Reference of 51114-68-2,Some common heterocyclic compound, 51114-68-2, name is 3-Chloro-2-methoxyaniline, molecular formula is C7H8ClNO, 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.
To a four-necked flask was added 30 g (0.19 mol) of 3-chloroanisidine,30 g (1.67 mol) of water was added and the temperature was raised to 50 C,A solution of 36% HC1231 g (2.28 mol)After incubation for 0.5 h,The temperature was lowered to 0 C, and 30% NaN0244 was slowly added dropwise.Diazotization reaction,Upon completion of the addition,After 2h incubation,Remove the filter cake. 69.5 g (0.38 mol) of 48% HBF4 solution was added dropwise to the filtrate,To carry out condensation reaction,Insulation lh later.The solution was filtered,The solids were dried for dehydration.The dried fluoroborate,Slowly heated to 130 C for cracking reaction,Until no gas is produced.After the cracking of the solution for distillation,The 2,6-CFA fraction was collected to give 26 g of the title compound. Purity> 98.5%,The yield of 3 steps was 85% (from 2,3-dichloronitrobenzene to the final target compound,The overall yield was 69.4%).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Chloro-2-methoxyaniline, its application will become more common.
Reference:
Patent; JIANG SU LIANHE CHEMICAL TECHNOLOGY CO LTD; LIANHE CHEMICAL TECHNOLOGY (YANCHENG )CO LTD; LIANHE CHEMICAL TECHNOLOGY (SHANGHAI )CO LTD; FAN, XIAOBIN; ZHANG, JUNTAO; XU, XIAOMING; WANG, HUI; YANG, JUN; SHEN, QIFU; (10 pag.)CN103787846; (2016); B;,
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