HRID2386681

反应详情

EQUATION

反应方程式

HRID 2386681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

TEA (0.84 mL, 6.04 mmol) was added to a solution of trans-3-amino-cyclopentanol (1.83 g) in anhydrous THF (10 mL), under argon atmosphere. 4-Chloro-2-methylsulfanyl-pyrimidine-5-carbonitrile (1.13 g, 6.04 mmol) was then added in two portions and the resulting mixture was stirred, at RT, under argon atmosphere, for 2 h. The liquid layer was decanted and THF was added to the gummy residue. The extraction procedure was repeated and the combined extracts were evaporated under reduced pressure. The crude residue was absorbed onto silica gel and purified by flash chromatography (EtOAc/hexane) to give 1.0 g of trans-4-(3-hydroxy-cyclopentylamino)-2-methylsulfanyl-pyrimidine-5-carbonitrile.

WORKUP

后处理

  1. customThe liquid layer was decanted
  2. additionTHF was added to the gummy residue
  3. extractionThe extraction procedure
  4. customthe combined extracts were evaporated under reduced pressure
  5. customThe crude residue was absorbed onto silica gel
  6. custompurified by flash chromatography (EtOAc/hexane)