반응 #62745

반응 방정식

Guanidine hydrochloride

sodium methoxide

guanidine

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

→

yellow solid

수율 42.8%

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

수율 42.8%

용매

methanol

methanol

반응 조건

후처리

1. 1
   여과the resultant sodium chloride was filtered
2. 2
   세척washed with methanol (10 mL)
3. 3
   온도the mixture heated
4. 4
   온도at reflux for 2 hr

실험 절차

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.

출처