HRID1521612
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
To a cooled (0° C.) solution of the title compound from Example 71 Step B (200 mg, 0.78 mmol) in tetrahydrofuran (3.9 mL) at 0° C. was added a solution of diisobutyl aluminum hydride in hexanes (1.0 M, 1.56 mL, 1.56 mmol). The reaction was warmed to room temperature and stirred overnight. Water and magnesium sulfate were then added, and the resulting suspension was stirred for 30 minutes, then filtered and concentrated under reduced pressure. Purification by flash chromatography on silica gel (20-100% ethyl acetate in hexanes) provided the title compound: LCMS m/z 229.67 [M+2+H]+; 1H NMR (500 MHz, CDCl3) δ 8.50 (s, 2H), 7.83 (s, 1H), 3.69 (s, 2H), 0.96-0.90 (m, 4H).
WORKUP
后处理
- stirringthe resulting suspension was stirred for 30 minutes
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customPurification by flash chromatography on silica gel (20-100% ethyl acetate in hexanes)