HRID1530646
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of 12-bromo-4-[3-methyl-1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene (1.0 g, 2.6 mmol), hexamethyldisilazane (3.0 mL, 14 mmol), and Pd(PPh3)2Cl2 (0.09 g, 0.13 mmol) in dry DMF (10 mL) was heated under CO atmosphere at 80° C. overnight. Most of the solvent was removed and water (20 mL) was added. The solid was collected by filtration, washed with water, and dried in vacuo to afford 4-[3-methyl-1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene-12-carboxamide (1.3 g, 95% yield) as a gray solid. LCMS (ESI) m/z: 353.3 [M+H+].
WORKUP
后处理
- customMost of the solvent was removed
- additionwater (20 mL) was added
- filtrationThe solid was collected by filtration
- washwashed with water
- customdried in vacuo