HRID23156

反应详情

EQUATION

反应方程式

HRID 23156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

4-Nitro-1H-pyrrole-2-carboxylic acid ethyl ester (5 g) was dissolved in 50 ml of dry EtOH, 50 ml of 1M sodium ethylate was added followed with 10 ml of CH3I. The reaction mixture was heated at 80° C. for 4 hours, cooled down to room temperature and distributed between water and chloroform. The organic phase was washed with water, dried with sodium sulfate and evaporated. The residue was recrystallized from hexane to yield 4.72 g (77%) of 1-propyl-4-nitro-1H-pyrrole-2-carboxylic acid ethyl ester 232. H1-NMR (DMSO-d6): 0.79 (t, 3H, CH3), 1.25 (t, 3H, CH3), 1.68 (m, 2H, CH2), 4.17-4.28 (m, 4H, 2CH2), 7.23 and 8.24 (d, 1H, pyrrole)

WORKUP

后处理

  1. temperaturecooled down to room temperature
  2. washThe organic phase was washed with water
  3. dry with materialdried with sodium sulfate
  4. customevaporated
  5. customThe residue was recrystallized from hexane