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
A solution of intermediate 17-5 (260 mg, 0.373 mmol) in DCE (400 mL) was bubbled through with N2 during 2 h. Hoveyda-Grubbs 1st generation catalyst (45 mg, 0.2 eq) was next added and the reaction mixture was heated at 80° C. under N2 overnight. The reaction mixture was then concentrated under reduced pressure and purified by flash chromatography (CH2Cl2/methanol 95:5) to give the desired product 18 as a gray powder after recrystallization from CH2Cl2/isopropyl ether; m/z=668 (M+H+), NMR (DMSO-d6): δ (ppm) 1.20-1.30 (m, 3H), 1.63-1.93 (m, 9H), 2.34 (m, 2H), 2.66 (m, 1H), 2.67 (s, 3H), 2.73 (s, 3H), 3.23 (m, 2H), 4.50 (s, 2H), 5.64 (m, 2H), 7.45 (m, 1H), 7.73-8.12 (m, 6H), 8.47 (broad s, 1H, NHCO), 8.54 (d, J=8.4 Hz, 1H), 11.47 (broad s, 1H, NHSO2).
WORKUP
后处理
- concentrationThe reaction mixture was then concentrated under reduced pressure
- custompurified by flash chromatography (CH2Cl2/methanol 95:5)