HRID2416533

反应详情

EQUATION

反应方程式

HRID 2416533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of (2E)-3-[4-(2-pyrimidinyl)phenyl]-2-propen-1-ol (300 mg, 1.41 mmol, prepared as described in Reference Example 65), ammonium formate (445 mg, 7.06 mmol), and 10% Pd/C (100 mg) in methanol (5 mL) was stirred for 1 h at room temperature. Solids were removed by filtration through Celite and washed with additional methanol (20 mL). The filtrate was concentrated and the residue was taken up in ethyl acetate (30 mL), washed with water (20 mL), dried (MgSO4) and concentrated. Purification by chromatography (SiO2, 1:1 dichloromethane/ethyl acetate) provided 240 mg (79%) of the title compound as a colorless oil. MS 215 (M+H)+.

WORKUP

后处理

  1. customSolids were removed by filtration through Celite
  2. washwashed with additional methanol (20 mL)
  3. concentrationThe filtrate was concentrated
  4. washwashed with water (20 mL)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customPurification by chromatography (SiO2, 1:1 dichloromethane/ethyl acetate)