反応 #62745

反応方程式

Guanidine hydrochloride

sodium methoxide

guanidine

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

→

yellow solid

収率 42.8%

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

収率 42.8%

溶媒

methanol

methanol

反応条件

後処理

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

実験手順

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.

出典