反应 #1135797

ord-dcc38955e6714627b69d85307b2d3c3a

反应方程式

COC(=O)Cl
methyl chloroformate
C1CCOC1
tetrahydrofuran
Cc1c(N)cccc1Cl
1-chloro-2-methyl-3-aminobenzene
COC(=O)Nc1cccc(Cl)c1C
1-chloro-2-methyl-3-methoxycarbonylaminobenzene

溶剂

反应条件

温度
25°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他To the reaction mixtures
  2. 2
    萃取the resulting mixtures were extracted with ethyl acetate
  3. 3
    洗涤The organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    干燥were dried over anhydrous sodium sulfate
  5. 5
    浓缩The mixtures were concentrated under reduced pressure

实验过程

Under cooling, to a mixture of methyl chloroformate 30 mL and tetrahydrofuran 50 mL was added dropwise 1-chloro-2-methyl-3-aminobenzene 5.00 g and the mixtures were stirred at 25° C. for a half hour. To the reaction mixtures was added water and the resulting mixtures were extracted with ethyl acetate. The organic layers were washed with aqueous saturated sodium bicarbonate solution and were dried over anhydrous sodium sulfate. The mixtures were concentrated under reduced pressure to give 1-chloro-2-methyl-3-methoxycarbonylaminobenzene 5.80 g.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09380782B2uspto-grants-2016_07