HRID1515501
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
- 100 °C
PROCEDURE
实验过程
A mixture of 3-amino-4-methylbenzamide (75 mg, 0.5 mmol), 3,4-dimethoxyphenylboronic acid (91 mg, 0.5 mmol) and glyoxylic acid monohydrate (46 mg, 0.5 mmol) in acetonitrile (2.0 mL) and DMF (0.2 mL) was heated at 100° C. for 20 min in a microwave reactor. After removal of solvent, the crude was triturated with methylene chloride. The precipitate formed was collected by filtration and washed with methylene chloride to give 5A after drying. 1H NMR (400 MHz, Methanol-d4) δ ppm 3.79 (s, 3H) 3.81 (s, 3H) 5.15 (s, 1H) 6.91 (d, J=8.35 Hz, 1H) 6.95 (s, 1H) 7.05-7.14 (m, 4H); LC-MS 345 (M+H).
WORKUP
后处理
- customAfter removal of solvent
- customthe crude was triturated with methylene chloride
- customThe precipitate formed
- filtrationwas collected by filtration
- washwashed with methylene chloride