HRID1762074

反应详情

EQUATION

反应方程式

HRID 1762074 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the ethyl carbamate of 1-amino-2-cyanocyclohept-1-ene (11.6 g), o-fluorobenzhydrazide (8.74 g) and 1-methyl-2-pyrrolidone (140 mL) is stirred at reflux under nitrogen for 18 hours, cooled and triturated with water to produce solid material. It is recrystallized from (±)1-methoxy-2-propanol to afford pure 2-(2-fluorophenyl)-8,9,10,11-tetrahydro-7H-cyclohepta[e][1,2,4]triazolo-[1,5-c]pyrimidin-5(6H)one, m.p. 257°-259°, in 63% yield.

WORKUP

后处理

  1. temperatureat reflux under nitrogen for 18 hours
  2. temperaturecooled
  3. customtriturated with water
  4. customto produce solid material
  5. customIt is recrystallized from (±)1-methoxy-2-propanol