反応 #1135797

ord-dcc38955e6714627b69d85307b2d3c3a

反応方程式

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

溶媒

反応条件

温度
25°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他To the reaction mixtures
  2. 2
    抽出the resulting mixtures were extracted with ethyl acetate
  3. 3
    洗浄The organic layers were washed with aqueous saturated sodium bicarbonate solution
  4. 4
    乾燥were dried over anhydrous sodium sulfate
  5. 5
    濃縮The mixtures were concentrated under reduced pressure

実験手順

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.

出典

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