反应 #987305

反应方程式

phenylenediamine

3,3-diethoxyacrylic acid ethyl ester

→

4-ethoxy-1,3-dihydro-benzo[b][1,4]diazepin-2-one

收率 56.5%

溶剂

acetic acid

—

xylenes

—

xylenes

反应条件

后处理

1. 1
   温度was cooled to room temperature
2. 2
   过滤The resulting white precipitate was filtered
3. 3
   洗涤was washed with ether (100 mL)
4. 4
   其他was dried under vacuum

实验过程

To a solution phenylenediamine (17.2 g, 159.2 mmol) and acetic acid (0.4 mL) in xylenes (225 mL) at 140° C. was added 3,3-diethoxyacrylic acid ethyl ester (30.0 g, 159.2 mmol) in xylenes (80 mL) dropwise over 50 minutes. The reaction was heated at 140° C. for 2 hours, was cooled to room temperature, and was stirred for 24 h. The resulting white precipitate was filtered, was washed with ether (100 mL), and was dried under vacuum to provide 18.37 g of 4-ethoxy-1,3-dihydro-benzo[b][1,4]diazepin-2-one as a white fluffy solid. MS 205 (M+1).

来源