HRID911343
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Add 1M lithium aluminum hydride in THF (7.3 mL) to benzo[b]thiophene-6-carbonitrile (0.6 g, 3.6 mmol) at 0° C. in THF (36 mL). After 15 h at ambient temperature, cool to 0° C. and add sequentially water (1.82 mL), 2N aqueous NaOH (1.82 mL) and water (2.60 mL). Filter the solid and evaporate the filtrate to obtain the crude amine. Purify by SCX chromatography. Rinse the column with methanol, add a solution of the crude amine in methanol, wash the column with methanol and then elute with 1N ammonia in methanol. Concentrate in vacuo to give the title compound (0.55 g, 92%).
WORKUP
后处理
- filtrationFilter the solid
- customevaporate the filtrate
- customto obtain the crude amine
- customPurify by SCX chromatography
- washRinse the column with methanol
- additionadd a solution of the crude amine in methanol
- washwash the column with methanol
- washelute with 1N ammonia in methanol
- concentrationConcentrate in vacuo