反応 #7726

反応方程式

sodium methoxide

7-(3-Fluoro-benzyloxy)-2-methyl-3H-quinazolin-4-one

2-amino-4-(3-fluoro-benzyloxy)-benzoic acid

ethyl acetamidate HCl

ethyl acetamidate HCl

sodium methoxide

→

title compound

収率 97.0%

2-[7-(3-Fluoro-benzyloxy)-2-methyl-4-oxo-4H-quinazolin-3-yl]-acetamide

収率 97.0%

溶媒

water

methanol

反応条件

後処理

1. 1
   温度the resulting mixture was heated
2. 2
   温度under reflux for 19 h
3. 3
   温度the resulting mixture heated for another 1 h
4. 4
   ろ過filtered off

実験手順

7-(3-Fluoro-benzyloxy)-2-methyl-3H-quinazolin-4-one: To a mixture of 2-amino-4-(3-fluoro-benzyloxy)-benzoic acid (2.0 g, 7.7 mmol) and ethyl acetamidate HCl (1.9 g, 15.3 mmol) in methanol (30 mL) was added sodium methoxide (5.4 M, 0.83 g, 15.3 mmol) and the resulting mixture was heated under reflux for 19 h. After this time ethyl acetamidate HCl (1.9 g, 15.3 mmol) and sodium methoxide (5.4 M, 0.83 g, 15.3 mmol) was added and the resulting mixture heated for another 1 h. After cooling to rt the mixture was poured into water (40 mL) and then the resulting precipitate was stirred for 2 h, and filtered off to afford the title compound (2.1 g, 97%) as an off-white solid. MS: m/e=283.1 (M−H).

出典