تفاعل #62740

معادلة التفاعل

2-(7,8-Dimethoxy-2H-1-benzopyran-5-ylmethyl)-3-morpholino acrylonitrile

aniline hydrochloride

guanidine hydrochloride

sodium methoxide

→

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

المردود 42.7%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction was cooled
2. 2
   درجة الحرارةAfter continued reflux
3. 3
   أخرىthe product crystallized from the cooled reaction mixture
4. 4
   ترشيحFiltration
5. 5
   غسيلwash (2 L)

الإجراء التجريبي

2-(7,8-Dimethoxy-2H-1-benzopyran-5-ylmethyl)-3-morpholino acrylonitrile (562 g, 1.64 mol) and aniline hydrochloride (234 g, 1.80 mol) were refluxed in SD3A (2.4 L) for one hour. The reaction was cooled, and guanidine hydrochloride (313 g, 3.28 mol) and sodium methoxide (275 g, 5.08 mol) were added. After continued reflux, the product crystallized from the cooled reaction mixture. Filtration followed by water wash (2 L) gave 2,4-diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine (220 g, 42.7%). Crystallization from ethanol-water gave title compound, mp 235°-238°, identical to the product of Example 1C.

المصدر