HRID623759

反应详情

EQUATION

反应方程式

HRID 623759 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

(3-(4-Chlorophenyl)-4-methyl-5-(trifluoromethyl)-1H-pyrrol-2-yl)(morpholino)methanone (80 mg, 0.215 mmol) was dissolved in dry MeCN (5 mL). The solution was mixed with K2CO3 (59 mg, 0.429 mmol), followed by addition of 3-chlorobenzyl bromide (31 μL, 0.236 mmol). The reaction mixture was stirred vigorously at 80° C. overnight. The temperature was lowered to room temperature; the reaction mixture was combined with a few lumps of ice, Et2O (50 mL) and H2O (10 mL) to result in a clear two phase system. The phases were separated; the organic phase was washed with brine. Drying (Na2SO4) was followed by concentration in vacuo. The residue was dissolved in MeCN (30 mL), concentrated in vacuo and used for preparative TLC (silica, heptane/EtOAc, 5:1), providing 96 mg (90%) of SC-25 as a fluffy white solid.

WORKUP

后处理

  1. customwas lowered to room temperature
  2. customto result in a clear two phase system
  3. customThe phases were separated
  4. washthe organic phase was washed with brine
  5. dry with materialDrying (Na2SO4)
  6. concentrationwas followed by concentration in vacuo
  7. dissolutionThe residue was dissolved in MeCN (30 mL)
  8. concentrationconcentrated in vacuo
  9. customproviding 96 mg (90%) of SC-25 as a fluffy white solid