تفاعل #79061

معادلة التفاعل

NEt3

7-amino-4-thiono-3H-pyrido[4,3-d]pyrimidine

MeI

→

7-amino-4-methylthiopyrido[4,3-d]pyrimidine

المردود 68.2%

المذيبات

DMSO

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGAfter the two phases have been stirred for 20 min
2. 2
   workup.ADDITIONthe reaction mixture is poured
3. 3
   درجة الحرارةAfter further cooling at 0° C.
4. 4
   ترشيحthe solid is collected by suction filtration
5. 5
   أخرىdried in a vacuum oven

الإجراء التجريبي

NEt3 (6 mL, 43 mmol) is added to a solution of 7-amino-4-thiono-3H-pyrido[4,3-d]pyrimidine (0.77 g, 4.3 mmol) in DMSO (7 mL) stirred under N2 at 25° C. After the two phases have been stirred for 20 min, MeI (0.26 mL, 4.2 mmol) is added. After 2 h, the reaction mixture is poured onto stirring ice-water. Solid forms instantly. After further cooling at 0° C., the solid is collected by suction filtration and dried in a vacuum oven to give 7-amino-4-methylthiopyrido[4,3-d]pyrimidine (0.564 g, 68%). 1H NMR (DMSO) δ 8.98 (1H, s), 8.71 (1H, s), 6.94 (2H, brs), 6.49 (1H, s) 2.63 (3H, s).

المصدر