HRID1839668

反应详情

EQUATION

反应方程式

HRID 1839668 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
92.5 °C

PROCEDURE

实验过程

A mixture of 3,5-dimethyl-1H-pyrrole-2-carbaldehyde (1.85 g, 15 mmol), dimorpholine-methane (5 mL, 27 mL) in THF (40 mL), water (15 mL) and acetic acid (4 mL) was heated to reflux (oil bath 90-95° C.) for 6 hours. The reaction was concentrated to a volume of 20 mL, basified with Na2CO3 and extracted with ethyl acetate (3×75 mL). The combined extracts were dried, concentrated and the residue was purified on a silica gel column to give 2 g (36%) of 3,5-dimethyl-4-morpholin-4-ylmethyl-1H-pyrrole-2-carbaldehyde as a solid.

WORKUP

后处理

  1. temperaturewas heated
  2. concentrationThe reaction was concentrated to a volume of 20 mL
  3. extractionextracted with ethyl acetate (3×75 mL)
  4. customThe combined extracts were dried
  5. concentrationconcentrated
  6. customthe residue was purified on a silica gel column