HRID928596

反应详情

EQUATION

反应方程式

HRID 928596 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of methyl 4-chloro-5-phenyl-thieno[2,3-d]pyrimidine-6-carboxylate (3.231 g, 10.59 mmol) and DIPEA (2.39 mL, 15.89 mmol) in THF (60 mL) at room temperature was added nortropine (1.682 g, 15.89 mmol) and the reaction left to stir overnight. The reaction was diluted with water (60 mL) and the layers separated. The aqueous layer was acidified to pH 3 and extracted repeatedly with 3:1 chloroform/IPA. The combined organic layers were dried over sodium sulphate, filtered and concentrated under reduced pressure to afford methyl 4-(3-hydroxy-8-azabicyclo[3.2.1]octan-8-yl)-5-phenyl-thieno[2,3-d]pyrimidine-6-carboxylate (1.839 g, 44%). LCMS: Rt=4.23, 396 (M+1).

WORKUP

后处理

  1. waitthe reaction left
  2. customthe layers separated
  3. extractionextracted repeatedly with 3:1 chloroform/IPA
  4. dry with materialThe combined organic layers were dried over sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure