HRID1911540

反应详情

EQUATION

反应方程式

HRID 1911540 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred mixture of (R)-2-amino-3-phenylsulfanyl-propan-1-ol (0.09 g, 0.49 mmol) and K2CO3 (0.081 g, 0.59 mmol) in THF (3 ml) under an argon atmosphere was added a solution of cyanogen bromide (0.062 g, 0.59 mmol) in THF (1 ml). The mixture was stirred overnight, then ethyl acetate and water were added. The aqueous phase was back-extracted with EtOAc. The combined organics were dried over MgSO4, filtered and concentrated. The crude product was purified by column chromatography (column: Isolute® Flash-NH2 from Separtis; eluent: EtOAc/MeOH=95:5) to yield a light yellow solid, (0.026 g, 26%); MS (ISP): 209.1 ((M+H)+.).

WORKUP

后处理

  1. extractionThe aqueous phase was back-extracted with EtOAc
  2. dry with materialThe combined organics were dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude product was purified by column chromatography (column: Isolute® Flash-NH2 from Separtis; eluent: EtOAc/MeOH=95:5)
  6. customto yield a light yellow solid, (0.026 g, 26%)