HRID266895

反应详情

EQUATION

反应方程式

HRID 266895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred solution of the spiro[2H-1-benzopyran-2,4'-piperidin]-4(3H)-one, hydrochloride (53 mg, 0.21 mmol) in methanol (5 mL) at 0° C., was added sodium borohydride (38 mg, 1 mmol) in several portions. After 30 minutes the mixture was evaporated and then treated with concentrated hydrochloric acid (2 mL) for 30 min. Evaporation gave a residue which was hydrogenated with palladium on carbon (10%, 10 mg), H2 (1 atm) in ethanol for two hours. Filtration to remove the catalyst gave the crude intermediate (89 mg) which was used without further purification.

WORKUP

后处理

  1. customAfter 30 minutes the mixture was evaporated
  2. additiontreated with concentrated hydrochloric acid (2 mL) for 30 min
  3. customEvaporation
  4. customgave a residue which
  5. filtrationFiltration
  6. customto remove the catalyst