反应 #62745

反应方程式

Guanidine hydrochloride

sodium methoxide

guanidine

3-(7,8-dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile

→

yellow solid

收率 42.8%

2,4-Diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine

收率 42.8%

溶剂

methanol

methanol

反应条件

后处理

1. 1
   过滤the resultant sodium chloride was filtered
2. 2
   洗涤washed with methanol (10 mL)
3. 3
   温度the mixture heated
4. 4
   温度at reflux for 2 hr

实验过程

Guanidine hydrochloride (11.46 g, 0.12 mole) in methanol (25 mL) was added to sodium methoxide (6.55 g, 0.12 mole) in methanol (40 mL) and the resultant sodium chloride was filtered and washed with methanol (10 mL). The guanidine solution was added to 3-(7,8-dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile (11.5 g, 0.04 mole) and the mixture heated at reflux for 2 hr. Cooling the mixture at 3° C. provided 5.38 g of yellow solid in two crops. HPLC assayed yield of 28.6%. A sample recrystallized from alcohol/water gave mp 232°-4° C.

来源