HRID1833256

反应详情

EQUATION

反应方程式

HRID 1833256 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
230 °C

PROCEDURE

实验过程

Concentrated sulfuric acid (0.4 mL) was added the mixture of [2-Cyano-2-(3,4-dimethoxy-phenyl)-vinyl]-carbamic acid ethyl ester (33.5 g, 121 mmol) and diphenyl ether (230 mL). The mixture was heated to 230° C. for 6 hr. After cooling, ether was added to precipitate the solid. The resulting solid was collected by filtration, washed with ether and dried to afford 6,7-Dimethoxy-1-oxo-1,2-dihydro-isoquinoline-4-carbonitrile (20.7 g, 74.1%) as a brown solid which was used without further purification. LC-MS m/e calcd for C12H10N2O3 (MH+) 231, found 231.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customto precipitate the solid
  3. filtrationThe resulting solid was collected by filtration
  4. washwashed with ether
  5. customdried