Tag: M.W=200-300

Reference of 14862-52-3, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 14862-52-3, name is 3,5-Dibromochlorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Toluene (200 ml) and water (50 ml)Of (9,9-dimethyl-9H-fluorene -2-yl) boronic acid (5.0 g, 21.0 mmol), 1,3-dibromo-5-chlorobenzene (14.19 g, 52.5 mmol), Pd (PPh3 ) it is refluxed in a solution of 4 (0.49 g, 0.42 mmol), and K2CO3 (5.80 g, 42.0 mmol) under nitrogen for 18 hours. After cooling to room temperature (~ 22 ), isolating the organic layer it was distilled off excess 1,3-dibromo-5-chlorobenzene. The residue as eluent heptane / DCM (9/1, v / v) for purification by column chromatography on silica gel, and as a colorless crystalline solid 2- (3-bromo-5-chlorophenyl) -9, 9-dimethyl -9H- FluoreneTo give a (6.2 g, 77%).

The chemical industry reduces the impact on the environment during synthesis 3,5-Dibromochlorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Universal Display Corporation; Cheng, Licang; Rayekh, Suman; Vaudreuil, Pierre Ruik-T; Elshennawy, Zaineb; Kottas, Greg; Diatkine, Alexei Borysovych; Joseph, Scott; Adamowicz, Vadim; Xia, Chuanjun; Wang, Ting Chiu; Jage, Walter; (109 pag.)KR2016/6633; (2016); A;,
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In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 61881-19-4 as follows. Computed Properties of C8H5ClF3N

X4 – 4 (594 mg, 1 mmol), N – benzene three fluorine second grades acyl chloride (0.45 ml, 3 mmol, 3 eq) dissolved in 8 ml of acetone, in batches adding potassium carbonate (410 mg, 3 mmol, 3 eq), stirring at room temperature 1 hour (TLC detection consumption end), filtering, the filtrate turns on lathe does, column to obtain white solid (601 mg, yield 79%)

According to the analysis of related databases, 61881-19-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanghai Pharmaceutical Industry Institute; China Pharmaceutical Industry Zongyuan; Lin Feng; Lu Rui; Xu Qiulong; Chen Jianli; Han Jine; (33 pag.)CN104231009; (2017); B;,
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Related Products of 6579-54-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

a) 2-{[(2-Morpholin-4-yl ethyl)carbamoyl]amino}-1,3-benzothiazol-6-yl 2,6-dichlorobenzenesulfonate may be prepared in the following manner:To a solution of 260 mg of 1-(6-hydroxy-1,3-benzothiazol-2-yl)-3-(2-morpholin-4-ylethyl)urea in 19.4 cm3 of aqueous 0.1N sodium hydroxide solution are added 209 mg of finely ground 2,6-dichlorobenzenesulfonyl chloride. After stirring for about 5 hours at a temperature in the region of 20 C., a further 70 mg of 2,6-dichlorobenzenesulfonyl chloride are added. After stirring for about 18 hours at the same temperature, the reaction mixture is concentrated under reduced pressure (13 kPa) to a volume of about 5 cm3. The suspension obtained is cooled for about one hour at a temperature in the region of 5 C. The solid is filtered off by suction, washed with three times 2 cm3 of water precooled to about 5 C., and dried under reduced pressure (13 kPa) over phosphorus pentoxide. 216 mg of 2-{[(2-morpholin-4-ylethyl)carbamoyl]amino}-1,3-benzothiazol-6-yl 2,6-dichlorobenzenesulfonate are thus obtained in the form of a cream-coloured powder, the characteristics of which are as follows:Melting point: melting at 130 to 135 C. (Koefler block)1H NMR spectrum at 300 MHz: from 2.33 to 2.47 (m, 6H); from 3.22 to 3.38 (masked m, 2H); 3.59 (m, 4H); 6.79 (broad t, J=5.5 Hz, 1H); 7.01 (dd, J=2.5 and 9.0 Hz, 1H); 7.56 (d, J=9.0 Hz, 1H); from 7.69 to 7.81 (m, 4H); 10.95 (broad m, 1H)Mass spectrum: LCMS: m/z 531: [M+H]+, m/z 529: [M-H]-

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2,6-Dichlorobenzenesulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; AVENTIS PHARMA S.A.; US2008/194555; (2008); A1;,
Chloride – Wikipedia,
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Electric Literature of 210532-25-5, These common heterocyclic compound, 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A mixture of 100 mg (0.32 mmol) E-11, 137 mg (0.65 mmol) 3,5-difluorobenzenesulfonyl chloride, 78 muL (0.97 mmol) pyridine and 5 mL DCM is stirred at RT over night. Water (2 mL) is added and the reaction mixture is extracted three times with 4 mL DCM. The combined organic phases are concentrated under reduced pressure and the crude product is purified with RP-HPLC (C18, 25-85% acetonitrile in water containing 0.1% formic acid). Yield: 99 mg (64%). HPLC-MS: M+H = 486; tR=1,18 min.

Statistics shows that 3,5-Difluorobenzene-1-sulfonyl chloride is playing an increasingly important role. we look forward to future research findings about 210532-25-5.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; The designation of the inventor has not yet been filed; EP2546249; (2013); A1;,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 41965-95-1, name is 3-Chloro-4-methoxybenzylamine Hydrochloride, A new synthetic method of this compound is introduced below., SDS of cas: 41965-95-1

2-Amino-4-chlorobenzoic acid (1.0 g; 5.83 mmol), 15 ml of dry DCM, and TEA (4.87 ml; 35.0 mmol) were placed in a reaction flask under nitrogen. 3-Chloro-4- methoxybenzylamine hydrochloride (1.213 g; 5.83 mmol) was added slowly and then T3P (6.87 ml; 1 1.66 mmol; 50 % in EtOAc) was added keeping the temperature at rt. The mixture was stirred at rt overnight. The reaction mixture was diluted with DCM and washed three times with water. The organic phase was dried with a phase separator and evaporated to dryness to yield 1.58 g of 2-amino-4-chloro-N-(3-chloro-4-methoxybenzyl)benzamide. LC-MS (ES) [M+l]: 327.1.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; ORION CORPORATION; PRUSIS, Peteris; HOeGLUND, Lisa; TOeRMAKANGAS, Olli; HIETANEN, Ari; ARVELA, Riina; VESALAINEN, Anniina; HEIKKINEN, Terhi; WO2015/169999; (2015); A1;,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 57310-39-1, name is 3-Bromo-4-chlorotoluene, A new synthetic method of this compound is introduced below., Quality Control of 3-Bromo-4-chlorotoluene

General procedure: A mixture of bromotoluene intermediate 7-14 or 16 (10 mmol), N-bromosuccinimide (15 mmol, 2.67 g) and azobisisobutyronitrile (5 mmol, 82 mg) in tetrachloromethane (20 mL) was refluxed for 16 h. After cooling the mixture was filtered, the filtrate was diluted with dichloromethane (30 mL), washed with water (50 mL) and brine (50 mL), dried over anhydrous Na2SO4 and evaporated. The residue containing the adequate benzyl bromide derivative without further purification was used to the next step.

The synthetic route of 57310-39-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Szyma?ska, Ewa; Cha?upnik, Paulina; Szczepa?ska, Katarzyna; Cunado Moral, Ana Maria; Pickering, Darryl S.; Nielsen, Birgitte; Johansen, Tommy N.; Kie?-Kononowicz, Katarzyna; Bioorganic and Medicinal Chemistry Letters; vol. 26; 22; (2016); p. 5568 – 5572;,
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Reference of 823-57-4, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 823-57-4, name is 2-Bromo-5-chloroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

HCl (500ml) for 2-bromo-5-chloroaniline (50 g, 242.16 mmol) and the mixture stirred at 0 while NaNO2 (17.5g, 253.62 mmol) to H2O (50ml) was added dropwise dissolved in a -10 after 1 hour It was stirred. The KI (44.2g, 266.26mmol) was stirred was dropwise added, dissolved in H2O (50ml) one hour at 0 . After completion of the reaction with ethyl acetate and filter the solidExtracts were dried over MgSO4 and the organic layer was filtered under reduced pressure. The filtered organic layer was evaporated under reduced pressure to a rear purified by column chromatography to the desired compound 1-bromo-4-chloro-2-iodobenzene (62 g,Yield: 66%) was obtained.

The synthetic route of 2-Bromo-5-chloroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Doosan Corporation; Kim, Tae Hyung; Bae, Hyung Chan; Lee, Chang Jun; Sin, Jin Yong; Jo, Hyun Chong; Baek, Young Mi; Rah, Jong Gyu; Park, Ho Chul; (46 pag.)KR2015/8658; (2015); A;,
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Related Products of 60811-21-4, These common heterocyclic compound, 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

[00367] Synthesis of 5-bromo-3-chloro-2-fluorobenzaldehyde (26): 4-Bromo-2-chloro- 1-fluorobenzene (25, 16 g, 76.5 mmol) was dissolved in 50 mL of THF. The reaction mixture was cooled down to -78 C. A solution of LDA in THF (2 M, 38.2 mL, 76.4 mmol) was added dropwise over 20 min. The reaction mixture was stirred at -78 C for 10 min. DMF (8.4 mL) was added dropwise. The reaction mixture was allowed to warm -20 C, quenched with 30 mL of saturated ammonium chloride aqueous solution and extracted with methyl fei -butyl ether (50 mL X 3). The combined organic layers were washed with brine, dried over anhydrous Na2S04, and concentrated under reduced pressure to give crude product, which was purified by silica gel chromatography (5-10% EtOAc/petroleum ether) to afford 8.4 g of 5-bromo-3-chloro-2-fluorobenzaldehyde (26) as white solid (yield: 46%). 1H MR (400 MHz, OMSO-d6) delta 10.10 (s, 1H), 8.26 (s, 1H), 7.93 (s, 1H).

Statistics shows that 4-Bromo-2-chloro-1-fluorobenzene is playing an increasingly important role. we look forward to future research findings about 60811-21-4.

Reference:
Patent; KARYOPHARM THERAPEUTICS INC.; BALOGLU, Erkan; SHACHAM, Sharon; SENAPEDIS, William; (155 pag.)WO2017/31204; (2017); A1;,
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Related Products of 38762-41-3,Some common heterocyclic compound, 38762-41-3, name is 4-Bromo-2-chloroaniline, molecular formula is C6H5BrClN, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

A. Tert-butyl N-(4-bromo-2-chlorophenyl)carbamate A solution of 4-bromo-2-chloroaniline (5.00 g, 0.0242 mol) in tetrahydrofuran (50 mL) was reacted with a 1.0 M solution of sodium bis(trimethylsilyl)amide in tetrahydrofuran (53.2 mL, 0.0532 mol). The mixture was stirred 15 minutes at ambient temperature. Di-tert-butyl dicarbonate (6.34 g, 0.0290 mol) was added and the solution was stirred for 2 hours. The solvent was removed in vacuo, and the crude material was purified by flash column chromatography on silica using heptane /ethyl acetate (4:1). The solvent was removed in vacuo to give tert-butyl N-(4-bromo-2-chlorophenyl)carbamate as a white solid (4.214 g, 0.0137 mol). 1H NMR (DMSO-d6, 400 MHz) delta 8.75 (s, 1H), 7.71 (d, 1H), 7.54 (d, 1H), 7.50 (dd, 1H), 1.46 (s, 9H); TLC (heptane/ethylacetate 4:1) Rf 0.54.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Bromo-2-chloroaniline, its application will become more common.

Reference:
Patent; Abbott Laboratories; US2002/156081; (2002); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

823-57-4, name is 2-Bromo-5-chloroaniline, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Formula: C6H5BrClN

Step 2: Preparation of Compound a26 (0680) (0681) To a solution of Compound a25 (1 g, 4.84 mmol) in pyridine (8 mL) was added sodium hydride (0.21 g, 5.33 mmol) and acetyl chloride (0.42 ml, 5.81 mmol), and the solution was stirred at 80° C. for 1 hour. To the reaction solution was added water, and the solution was extracted with ethyl acetate twice. The organic layer was washed with water and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. To a solution of the obtained residue in THF/methanol (1:1, 9 ml) was added 2 mol/L sodium hydroxide aqueous solution (2.6 ml, 5.16 mmol), and the solution was stirred at room temperature for 30 minutes. To the reaction solution was added water, and the solution was extracted with ethyl acetate twice. The organic layer was washed with water and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. To the obtained residue was added ethyl acetate (5 ml), and the mixture was dissolved in a water bath of 80° C. After cooled to room temperature, hexane (5 ml) was added to the solution, and the precipitated solid was filtered, washed with isopropyl ether (5 ml), and dried under reduced pressure to Compound a26 (674.4 mg, yield: 53percent) as a pale brown solid. (0682) 1H-NMR (CDCl3) delta: 8.46 (s, 1H), 7.59 (s, 1H), 7.45 (d, 1H, J=8.5 Hz), 6.97 (d, 1H, J=8.5 Hz), 2.25 (s, 3H).

The synthetic route of 823-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The University of Tokyo; TOHOKU UNIVERSITY; Shionogi & Co., Ltd.; NAGANO, Tetsuo; OKABE, Takayoshi; KOJIMA, Hirotatsu; KAWAGUCHI, Mitsuyasu; NUREKI, Osamu; ISHITANI, Ryuichiro; NISHIMASU, Hiroshi; AOKI, Junken; TANAKA, Nobuyuki; KANDA, Yasuhiko; KIOI, Yoshiyuki; TATENO, Yusuke; KIDA, Shiro; YAMANE, Junji; (163 pag.)US2017/158704; (2017); A1;,
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