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
- 80 °C
PROCEDURE
实验过程
Pd2(dba)3 (9.2 mg, 0.01 mmol) was added to a mixture of tert-butyl 4-(6-bromo-1-methyl-1H-pyrrolo[3,2-c]pyridin-2-yl)-1H-pyrazole-1-carboxylate (28) (38 mg, 0.101 mmol), cesium carbonate (66 mg, 0.201 mmol), 3,4-dimethoxyaniline (18.5 mg, 0.121 mmol) and Xantphos (11.7 mg, 0.020 mmol) in dioxane (1.1 mL). The reaction mixture was heated at 80° C. for 19 hr. The reaction mixture was then filtered and the solution was concentrated under reduced pressure. The residue was purified by prep TLC (DCM/MeOH 95/5) to afford the title compound as a dark red solid (5 mg, 11%). 1H NMR (500 MHz, CDCl3) 1.71 (s, 9H), 3.50 (s, 1H), 3.89 (s, 1H), 3.91 (s, 1H), 6.48 (s, 1H), 6.57 (d, J=0.6 Hz, 1H), 6.64 (m, 1H), 6.89 (m, 2H), 6.92 (m, 1H), 7.91 (d, J=0.6 Hz, 1H), 8.26 (d, J=0.6 Hz, 1H), 8.49 (s, 1H).
WORKUP
后处理
- filtrationThe reaction mixture was then filtered
- concentrationthe solution was concentrated under reduced pressure
- customThe residue was purified by prep TLC (DCM/MeOH 95/5)