HRID1762074
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux under nitrogen for 18 hours
- temperaturecooled
- customtriturated with water
- customto produce solid material
- customIt is recrystallized from (±)1-methoxy-2-propanol