HRID1162782

反应详情

EQUATION

反应方程式

HRID 1162782 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

2-(2-Bromoacetamido)-N-(2-hydroxyethyl)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide (1.66 g, 4.60 mmol), 3-tert-butyl-1H-pyrazole-4-carbaldehyde (1.75 g, 11.49 mmol) and potassium carbonate (2.54 g, 18.38 mmol) were mixed with DMF (20 mL) and heated at 70° C. for 2 h. On cooling, the reaction was partitioned between EtOAc and water. The organics were washed with brine, dried over MgSO4 and concentrated directly onto silica for chromatographic purification (0-100% EtOAc/heptane). Concentration in vacuo yielded a white solid (1.64 g, 3.79 mmol, 83%).

WORKUP

后处理

  1. temperatureOn cooling
  2. customthe reaction was partitioned between EtOAc and water
  3. washThe organics were washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated directly onto silica for chromatographic purification (0-100% EtOAc/heptane)
  6. concentrationConcentration in vacuo