تفاعل #1764009

معادلة التفاعل

iodomethane

2-chloro-7,7-difluoro-9-(4-methoxy-benzyl)-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one

cesium carbonate

→

2-chloro-7,7-difluoro-9-(4-methoxy-benzyl)-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one

المردود 89.3%

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe mixture filtered
2. 2
   تركيزconcentrated under reduced pressure
3. 3
   workup.ADDITIONIce water was added to the residue
4. 4
   أخرىto give a precipitate
5. 5
   ترشيحThe solid was collected by filtration
6. 6
   غسيلwashed with water
7. 7
   أخرىdried under vacuum

الإجراء التجريبي

To a solution of 0.60 g (0.0017 mole) of 2-chloro-7,7-difluoro-9-(4-methoxy-benzyl)-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VI-291) in 8 mL of dimethylformamide was added 0.83 g (0.0026 mole) of cesium carbonate, followed by 0.32 mL (0.0051 mole) of iodomethane. After stirring four hours, the mixture filtered and then concentrated under reduced pressure. Ice water was added to the residue to give a precipitate. The solid was collected by filtration, washed with water and dried under vacuum to give 0.56 g of 2-chloro-7,7-difluoro-9-(4-methoxy-benzyl)-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VII-291) as a white solid.

المصدر