HRID1447424

反应详情

EQUATION

反应方程式

HRID 1447424 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.5 g (9.1 mmole) 8-chloro-4, 5-dihydro-5-methyl-4-oxopyrano[3,2-b]indole-2-carboxylic acid and 4.8 g (19.7 mmole) N-ethoxycarbonyl-2-ethoxy-1,2-dihydroquinoline (EEDQ) in 300 ml benzene was stirred for 45 min under nitrogen. To the reaction mixture was added 1.1 g (10.7 mmole) of 5-aminotetrazole monohydrate, and stirring was continued for a total of 88 hrs. The precipitate that had formed was filtered, stirred overnight in 50 ml of methanol, and refiltered. Two recrystallizations from DMF yielded a yellow solid of mp 300° C. dec.

WORKUP

后处理

  1. stirringstirring
  2. customwas continued for a total of 88 hrs
  3. customThe precipitate that had formed
  4. filtrationwas filtered
  5. stirringstirred overnight in 50 ml of methanol
  6. customTwo recrystallizations from DMF
  7. customyielded a yellow solid of mp 300° C. dec.