HRID1903069
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
To 75 ml of isopropanol is added 3.3 g (0.017 m) methyl 3-(2,3-dihydroxypropyl)amino-2-butenoate (3), 4.18 g (0.02 m) 5,6-dichloro-3-nitropyrazinamine (5), and 2.0 g (0.02 m) triethylamine. This solution is heated at 60°-65° for two days. The reaction mixture is then stripped on the rotary evaporator and the residue chromatographed on silica gel eluted with 12% methanol/chloroform. Material with Rf =0.5 is collected and after crystallization from acetonitrile the desired product is an orange solid, m.p. 184°-186° (dec).
WORKUP
后处理
- temperatureThis solution is heated at 60°-65° for two days
- customThe reaction mixture is then stripped on the rotary evaporator
- customthe residue chromatographed on silica gel
- washeluted with 12% methanol/chloroform
- customMaterial with Rf =0.5 is collected
- customafter crystallization from acetonitrile the desired product