Реакция #1135797

ord-dcc38955e6714627b69d85307b2d3c3a

Уравнение реакции

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

Растворители

Условия реакции

Температура
25°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеTo the reaction mixtures
  2. 2
    Экстракцияthe resulting mixtures were extracted with ethyl acetate
  3. 3
    ПромывкаThe organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    Сушкаwere dried over anhydrous sodium sulfate
  5. 5
    КонцентрированиеThe mixtures were concentrated under reduced pressure

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09380782B2uspto-grants-2016_07