HRID1601449

反应详情

EQUATION

反应方程式

HRID 1601449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Combine (S)-3-(2-(4-phenyl-4-carboxypiperidin-1-yl)ethyl)-3-(3,4-dichlorophenyl)pyrrolidine (50 g, 112 mmol) and sodium bicarbonate (30 g) in tetrahydrofuran (1300 mL) and water (300 mL). Add portionwise over about 45 minutes, a solution of 3,4,5-trimethoxybenzoyl chloride (26 g, 112 mmol) in tetrahydrofuran (130 mL). After 2 hours, dilute with water (1000 mL). Adjust the pH to about 4 using concentrated aqueous hydrochloric acid to give a solid. Collect the solid by filtration and rinse with water. Triturate the solid with methanol (1300 mL) and water (1300 mL). Filter, rinse with water and dry in vacuo to give the title compound.

WORKUP

后处理

  1. additionAdd portionwise over about 45 minutes
  2. customto give a solid
  3. customCollect the solid
  4. filtrationby filtration
  5. washrinse with water
  6. customTriturate the solid with methanol (1300 mL) and water (1300 mL)
  7. filtrationFilter
  8. washrinse with water
  9. customdry in vacuo