HRID911343

反应详情

EQUATION

反应方程式

HRID 911343 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationFilter the solid
  2. customevaporate the filtrate
  3. customto obtain the crude amine
  4. customPurify by SCX chromatography
  5. washRinse the column with methanol
  6. additionadd a solution of the crude amine in methanol
  7. washwash the column with methanol
  8. washelute with 1N ammonia in methanol
  9. concentrationConcentrate in vacuo