تفاعل #62745

معادلة التفاعل

Guanidine hydrochloride

sodium methoxide

guanidine

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

→

yellow solid

المردود 42.8%

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

المردود 42.8%

المذيبات

methanol

methanol

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe resultant sodium chloride was filtered
2. 2
   غسيلwashed with methanol (10 mL)
3. 3
   درجة الحرارةthe mixture heated
4. 4
   درجة الحرارةat reflux for 2 hr

الإجراء التجريبي

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.

المصدر