HRID1411532
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
- 110 °C
PROCEDURE
实验过程
A sealed tube equipped with a magnetic stirrer was charged with 118b (310 mg, 1 mmol), 3-(acetoxymethyl)-2-(1-oxo-3,4,6,7,8,9-hexahydropyrazino[1,2-a]indol-2(1H)-yl)pyridine-4-ylboronic acid 113i (385 mg, 1 mmol), Pd(dppf)Cl2 (80 mg, 0.1 mmol), K3PO4 (424 mg, 2 mmol), NaOAc (165 mg, 2 mmol), CH3CN (15 mL), and water (1 mL). After three cycles of vacuum/argon flush, the mixture was heated at 110° C. for 3 h. It was evaporated in vacuo. The residue was purified by silica gel column chromatography eluting with dichloromethane/methanol (50:1, V/V) to afford 118c (400 mg, 68%) as a yellow solid. LCMS: [M+H]+ 569
WORKUP
后处理
- customA sealed tube equipped with a magnetic stirrer
- customAfter three cycles of vacuum/argon flush
- customIt was evaporated in vacuo
- customThe residue was purified by silica gel column chromatography
- washeluting with dichloromethane/methanol (50:1, V/V)