Tag: M.W=100-200

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. 821-10-3, name is 1,4-Dichlorobut-2-yne, A new synthetic method of this compound is introduced below., Quality Control of 1,4-Dichlorobut-2-yne

1,4-Dichloro-2-butyne (16) (1.26 mL, 13.1 mmol) was added to a solution of malonate 15 (2.50 g, 8.73 mmol) and K2CO3 (3.62 g, 26.2mmol) in MeCN (60 mL) at room temperature. The reaction mixture was stirred for 12h at 90 C, and then H2O (30 mL) was added at 0 C. The resultant mixture was extracted with Et2O (30 mL×3), and the combined organic layers were dried over Na2SO4, filtered, and concentrated. The residue was purified by column chromatography on silica gel (30 g, n-hexane/EtOAc 4/1) to afford chloride 18 (2.54 g, 6.81mmol) in 78% yield.

The synthetic route of 821-10-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Masuda, Keisuke; Tanigawa, Masashi; Nagatomo, Masanori; Urabe, Daisuke; Inoue, Masayuki; Tetrahedron; vol. 73; 26; (2017); p. 3596 – 3605;,
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Application of 2401-24-3, A common heterocyclic compound, 2401-24-3, name is 2-Chloro-5-methoxyaniline, molecular formula is C7H8ClNO, 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.

EXAMPLE 48 4-(2-Chloro-5-methoxyanilino)-6-(methoxymethyl)-2-(2-methyl-1,3-thiazol-4-yl)pyrimidine The title compound was prepared from a mixture of 4-chloro-6-(methoxymethyl)-2-(2-methyl-1,3-thiazol-4-yl)pyrimidine (50 mg, 0.196 mmol) and 2-chloro-5-methoxyaniline (38 mg, 0.196 mmol) similar to Example 13 and isolated as a white solid (33 mg, 45%). 1H NMR (CDCl3): 8.14 (s, 1H), 7.93 (d, J=3.0 Hz, 1H), 7.32 (d, J=8.7 Hz, 1H), 7.22 (s, 1H), 6.86 (s, 1H), 6.64 (dd, J=3.0, 9.3 Hz, 1H), 4.60 (s, 2H), 3.88 (s, 3H), 3.52 (s, 3H), 2.84 (s, 3H).

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; Cytovia, Inc.; US2003/69239; (2003); A1;,
Chloride – Wikipedia,
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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. 67952-93-6, name is 3-Chloro-4-methylbenzylamine, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 67952-93-6

General procedure: Under an Ar atmosphere, to a solution of benzylamine 1a (0.55 mL, 5 mmol) in 20 mL of CH2Cl2, FeCl3 (811 mg, 5.0 mmol) and m-CPBA (2.2 g, 10.5 mmol, 85%) were added successively at 0 C. The reaction mixture was stirred at 0 C for 3h (TLC monitoring) and quenched with saturated aqueous Na2S2O3 (10 mL). Then, 10% NaOH solution (15 mL) and H2O (15 mL) were added and the mixture wasextracted with CH2Cl2. The combined extracts were dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using petroleum ether/ethyl acetate as eluant to give the light yellow liquid product of N,N-dichlorobenzylamine 2a 850 mg (97%).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 67952-93-6.

Reference:
Article; Liu, Jia; Xu, Junchao; Ren, Jiangmeng; Zeng, Bu-Bing; Chemistry Letters; vol. 43; 2; (2014); p. 190 – 192;,
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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. 104-77-8, name is 3-Chloro-N,N-diethylpropan-1-amine, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C7H16ClN

EXAMPLE 17 Methyl 2-(3-diethylamino-propyl)-5-(3,5-dichlorophenylamino)-2H-1,2,3-triazole-4-carboxylate hydrochloride A mixture consisting of 5.8 gm (0.02 mol) of methyl 1-(3,5-dichlorophenyl)-5-amino-1H-1,2,3-triazole-4-carboxylate, 80 ml of absolute dimethylformamide, 0.8 gm of sodium hydride dispersion and 3.0 gm (0.02 mol) of 1-chloro-3-diethylamino-propane was reacted and worked up as in Example 15. 0.9 gm (9.2% of theory) of the desired compound was obtained; melting point 158 C.

According to the analysis of related databases, 104-77-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Boehringer Ingelheim KG; US4505912; (1985); A;,
Chloride – Wikipedia,
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Related Products of 15205-11-5, A common heterocyclic compound, 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, molecular formula is C7H7ClFN, 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.

Example 38 N-[(2-chloro-4-fluorophenyl)methyl]-1-(2-methyl-2-propen-1-yl)-5-oxoprolinamide (E38) Crude 1-(2-methyl-2-propen-1-yl)-5-oxoproline (~0.075 g, ~0.41 mmol, prepared as described below) was dissolved in dichloromethane (5 ml) and to this was added 1-Hydroxybenzotriazole (0.061 g, 0.45 mmol), [(2-chloro-4-fluorophenyl)methyl]amine (0.068 g, 0.43 mmol), and N-(3-dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride (0.087 g, 0.45 mmol). The mixture was then stirred at room temperature for 24 hrs. The mixture was diluted with more dichloromethane then washed sequentially with 2M aqueous hydrogen chloride and saturated aqueous sodium hydrogen carbonate. The organic layer was filtered through a phase separator and evaporated to give a brown residue which was purified by mass-directed automated HPLC to give pure N-[(2-chloro-4-fluorophenyl)methyl]-1-(2-methyl-2-propen-1-yl)-5-oxoprolinamide (0.018 g) as a white solid. LC/MS [M+H]+=325.1, retention time=2.40 minutes.

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; GLAXO GROUP LIMITED; US2008/9541; (2008); A1;,
Chloride – Wikipedia,
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Some common heterocyclic compound, 6276-54-6, name is 3-Chloropropan-1-amine hydrochloride, molecular formula is C3H9Cl2N, 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. Safety of 3-Chloropropan-1-amine hydrochloride

Step-3: Synthesis of Compound 4 (0140) (0141) To a stirred suspension of crude (2R,3R,4S)-2,3,4,6-tetrakis(benzyloxy)-5-oxohexanal 3 (20 g, 37.13 mmol) in MeOH (400 mL) were added 3-chloro propylamine (47 g, 743 mmol) at 0 C. and activated molecular sieves (100 g) and the reaction mixture was stirred at room temperature for 20 min. Then the reaction mixture was cooled to 0 C. and solid NaBH3CN (9.33 g, 148.5 mmol) was added to the reaction mixture and stirred at same temperature for 1 h. Then the reaction mixture was stirred at room temperature for 20 h. After removal of the molecular sieves through celite pad, the filtrate was concentrated under reduced pressure. The crude mass was dissolved in ethyl acetate (250 mL) and organic part was washed with saturated solution of NaHCO3 (100 mL), dried over Na2SO4 and concentrated under reduced pressure to get crude which was purified by column chromatography using 100-200 mesh silica gel and eluting with 8% EtOAc/hexane to afford (2R,3R,4R,5S)-3,4,5-tris(benzyloxy)-2-[(benzyloxy)methyl]-1-(3-chloropropyl)piperidine 4 (8.0 g, 36%) as white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6276-54-6, its application will become more common.

Reference:
Patent; CELLIX BIO PRIVATE LIMITED; Kandula, Mahesh; US9150557; (2015); B1;,
Chloride – Wikipedia,
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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. 2163-00-0, name is 1,6-Dichlorohexane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 2163-00-0

Examples 2 to 5; The procedure of Example 1 was repeated, except that the reaction of 1,6-dichlorohexane was carried out at a constant pH of 5, 6, 8 and 9. Before the start of the particular reaction, the weakly acidic mixture was adjusted to the pH of 5, 6, 8 and 9 with 2.5% sodium hydroxide solution (measurement with pH electrodes). Example 2 Example 3 Example 4 Example 5 pH value in 5.0 +/- 0.1 6.0 +/- 0.1 8.0 +/- 0.1 9.0 +/- 0.1 the reaction Residual 1,6-dichloro- <10 <10 <10 approx. 11 hexane content (ppm) Conversion of 1,6- >99.9 >99.9 >99.9 >99.9 dichlorohexane (%) In all examples (Examples 2 to 5), the resulting reaction mixture was clear and homogeneous. To determine the pure yield with respect to Examples 2 and 5, they were repeated once more. However, a GC analysis sample was not taken from the particular reaction mixture. The pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate was approx. 91.4%2) for the repetition of Example 2 and approx. 90.6%2) for the repetition of Example 5. 2) The pure yield for the synthesis according to Examples 2 and 5 was carried out again as in Example 1 by reacting the reaction solutions obtained in each case with aqueous NaBEC solution. In this procedure, the yield of 1,6-bis(N,N-dibenzylthiocarbamoyldithio)hexane was approx. 89.6% of theory with a content of 95% for the reaction according to Example 2 and approx. 89.7% of theory with a content of approx. 94% for that according to Example 5. Thus, the pure yield of the (di)sodium salt (di)hydrate of hexamethylene 1,6-bisthiosulphate in the inventive reaction of 1,6-dichlorohexane with sodium thiosulphate pentahydrate must have been approx. 91.4% for the reaction according to Example 2 (89.6%×0.95×1/0.931=91.4%) and approx. 90.6% for that according to Example 5 (89.7%×0.94×1/0.931=90.6%).

The synthetic route of 2163-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Buding, Hartmuth; US2005/240044; (2005); A1;,
Chloride – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 1871-57-4, Quality Control of 3-Chloro-2-chloromethyl-1-propene

General procedure: To a cooled solution (5 C) of the corresponding 4,6-O-(R)-benzylidene-d-hexopyranoside derivative (obtained using the procedure describe by our group2c) (35.4 mmol) in dry THF (70 mL) were added, successively, freshly powdered potassium hydroxide (7.0 g, 125 mmol), 18-crown-6 (0.38 g, 1.4 mmol), and 3-chloro-2-chloromethylpropene (4.1 mL, 35.4 mmol). The reaction mixture was stirred at this temperature for 3 h, and left at room temperature until all the starting material had been consumed, as monitored by TLC (5-7 days, approximately), then diluted with dichloromethane (60 mL) and washed successively with water and aqueous saturated solution of sodium bicarbonate, dried (MgSO4), filtered, and the filtrate was evaporated to dryness.

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, 3-Chloro-2-chloromethyl-1-propene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Vega-Perez, Jose M.; Vega-Holm, Margarita; Perinan, Ignacio; Palo-Nieto, Carlos; Iglesias-Guerra, Fernando; Tetrahedron; vol. 67; 2; (2011); p. 364 – 372;,
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These common heterocyclic compound, 344-19-4, name is 2,6-Dichloro-4-fluoroaniline, 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. Formula: C6H4Cl2FN

Preparation 10 2,6 Dichloro-4-fluoro-phenylhydrazine hydrochlorideTo a 0 0C solution of 2,6 Dichloro-4-fluorophenylamine (3.0 g, 16.6 mmol) in 12 M HCl (30 mL) and TFA (20 mL) is added slowly and dropwise NaNO2 (20 mmol, 1.37 mL) in water (6 mL). The reaction is stirred at 0 0C for 1 h. A solution of SnCl2 (5.74 g, 25.6 mmol) in 12 M HCl (16 mL) is added over 15 minutes. The ice bath is removed and the reaction is stirred for 18 h. The reaction is filtered and the solid is washed with isopropyl alcohol. The solid is dried to yield the title compound (3.0 g, 96 %). LC-ES/MS m/e 194.0 (M+ 1)

The synthetic route of 2,6-Dichloro-4-fluoroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2007/140183; (2007); A1;,
Chloride – Wikipedia,
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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. 5013-77-4, name is N-Methyl-2,4-dichlorobenzylamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of N-Methyl-2,4-dichlorobenzylamine

General procedure: To a stirring solution of carboxylic acid (10 mmol, 1.0equiv) in dry DMF (10 mL) in a two-neck flask under argon atmosphere at -10 oC, HOBt (hydrate form, 1.76 g, 13 mmol,1.3 equiv) was added followed by the addition of DIPEA (2.26 mL, 13 mmol, 1.3 equiv) and EDCI (2.02 g, 13 mmol, 1.3equiv). The reaction mixture was stirred at -10 oC for 30 min before an appropriate amine (10 mmol, 1.0 equiv) was addedand allowed to warm to room temperature. After 16 h, the reaction mixture was treated with 10% citric acid solution (25mL) and extracted with DCM. The organic phase was washed with saturated NaHCO3 solution (2 ×), followed with waterand brine, dried over anhydrous Na2SO4, filtered, and evaporated in vacuo to remove solvents. The crude product waspurified by silica gel flash chromatography (EtOAc-Heptane).

The synthetic route of 5013-77-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Mai, Anh Hung; Pawar, Sonalika; De Borggraeve, Wim M.; Tetrahedron Letters; vol. 55; 33; (2014); p. 4664 – 4666;,
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