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
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
A mixture of (3R,3aR,6R,6aR)-6-(6-chloro-5-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)-3-(2-trimethylsilanyl-ethoxymethyl)-3H-imidazo[4,5-b]pyridin-2-yloxy)hexahydrofuro[3,2-b]furan-3-ol (1.00 g), N′-(4-bromophenyl)-N,N-dimethyl-methanesulfonimidamide (484 mg), Na2CO3 (2 M aqueous solution, 1.98 mL), and ethanol (8 mL) is purged for 5 minutes with argon. [1,1′-Bis(diphenylphosphino)-ferrocene]-dichloropalladium(II)-CH2Cl2-complex (PdCl2(dppf)×CH2Cl2) (130 mg) is added and the mixture is stirred over night at 70° C. The reaction mixture concentrated in vacuo and the residue is purified by preparative HPLC to give the title compound. LC (method 1): tR=1.13 min; Mass spectrum (ESI+): m/z=700 [M+H]+.
WORKUP
后处理
- customis purged for 5 minutes with argon
- addition[1,1′-Bis(diphenylphosphino)-ferrocene]-dichloropalladium(II)-CH2Cl2-complex (PdCl2(dppf)×CH2Cl2) (130 mg) is added
- concentrationThe reaction mixture concentrated in vacuo
- customthe residue is purified by preparative HPLC