HRID928596
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- waitthe reaction left
- customthe layers separated
- extractionextracted repeatedly with 3:1 chloroform/IPA
- dry with materialThe combined organic layers were dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure