反応 #53346

ord-334775d56d9c4fd4b1e9df895da9cc7d

反応方程式

CC1Cc2cc3c(cc2C(c2ccc([N+](=O)[O-])cc2)=NN1C(N)=S)OCO3
starting material I
CC1Cc2cc3c(cc2C(c2ccc([N+](=O)[O-])cc2)=NN1C(N)=S)OCO3
(±)-8-Methyl-5-(4-nitrophenyl)-7-thiocarbamoyl-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine
COC(=O)CBr
methyl bromoacetate
CN(C)C=O
dimethylformamide
CC1Cc2cc3c(cc2C(c2ccc([N+](=O)[O-])cc2)=NN1C1=NC(=O)CS1)OCO3
title compound
収率 91.0%
CC1Cc2cc3c(cc2C(c2ccc([N+](=O)[O-])cc2)=NN1C1=NC(=O)CS1)OCO3
(±)-7-(4,5-Dihydro-4-oxo-thiazol-2-yl)-8-methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine
収率 91.0%

溶媒

反応条件

温度
85°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他obtained crude product
  2. 2
    その他was purified
  3. 3
    温度by refluxing in methanol

実験手順

A mixture of 1.00 g (2.6 mmol) of the starting material I, 1.19 g (7.78 mmol) of methyl bromoacetate and 10 ml of dimethylformamide was stirred at 80-90° C. for 1 h. After diluting with water the obtained crude product was purified by refluxing in methanol to yield 1.00 g (91%) of the title compound; Mp.: 218-220° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06858605B2uspto-grants-2005_02