HRID520814

反应详情

EQUATION

反应方程式

HRID 520814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-[4-(1-t-Butyloxycarbonyl piperidin-4-yloxy)phenyl]-1-(morpholin-4-yl)prop-2-ene-1-one (29.8 grams, 0.071 moles) in dichloromethane (400 mL) was treated with trifluoroacetic acid (55.6 mL, 0.726 moles) at room temperature. The reaction mass was stirred for 6 hours at room temperature. The progress of the reaction was monitored by thin layer chromatography. After completion of the reaction, the reaction mass was poured on to chilled water (500 mL) and basified with 40% lye solution (pH˜9). The layers were separated and the aqueous layer was extracted with dichloromethane (2×200 mL) and the combined organic phase was washed with water (150 mL), brine solution (150 mL) and dried over sodium sulphate. The organic phase was concentrated on rotavacuum to afford the title compound (21.2 grams).

WORKUP

后处理

  1. customAfter completion of the reaction
  2. additionthe reaction mass was poured on
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with dichloromethane (2×200 mL)
  5. washthe combined organic phase was washed with water (150 mL), brine solution (150 mL)
  6. dry with materialdried over sodium sulphate
  7. concentrationThe organic phase was concentrated on rotavacuum