HRID2416533
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customSolids were removed by filtration through Celite
- washwashed with additional methanol (20 mL)
- concentrationThe filtrate was concentrated
- washwashed with water (20 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customPurification by chromatography (SiO2, 1:1 dichloromethane/ethyl acetate)