HRID715134
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
- 60 °C
PROCEDURE
实验过程
Treat a solution of prop-1-en-2-yl(2-fluoro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)carbamate (0.460 g, 1.432 mmol) in THF (5 mL) with cycloheptylamine (0.195 g, 1.719 mmol) followed by a catalytic amount of 1-methylpyrrolidine (0.012 g, 0.143 mmol) and heat at 60° C. for 2 h. Concentrate the mixture to dryness, add MeCN, collect the solid via filtration and dry to afford the title compound (420 mg, 78%) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ 8.50 (dd, J=9, 1.7 Hz, 1H), 8.33 (s, 1H), 7.16 (m, 2H), 6.60 (d, J=7.0 Hz, 1H), 3.64 (m, 1H), 1.80 (m, 2H), 1.50 (m, 10H), 1.26 (s, 12H); MS(ESI) m/z: 377.2 (M+H+).
WORKUP
后处理
- concentrationConcentrate the mixture to dryness
- additionadd MeCN
- customcollect the solid
- filtrationvia filtration
- customdry