تفاعل #3638

معادلة التفاعل

9-oxo-9,10-dihydro-4H-pyrrolo[1,2-a]thieno[2,3-e][1,4]diazepin

boron dimethylsulfide

methanol

→

desired product

9,10-Dihydro-4H-pyrrolo[1,2-a]thieno[2,3-e][1,4]diazepine

المذيبات

tetrahydrofuran

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture is refluxed for 6 hours
2. 2
   أخرىThe volatiles are removed under vacuum
3. 3
   workup.ADDITIONTo the residue is added 100 ml of 2N NaOH
4. 4
   درجة الحرارةThe mixture is refluxed 5 hours
5. 5
   ترشيحfiltered
6. 6
   استخلاصThe solid is extracted with dichloromethane
7. 7
   غسيلthe extract is washed with 2N citric acid, water
8. 8
   تجفيفdried (Na2SO4)
9. 9
   أخرىThe solvent is removed in vacuo

الإجراء التجريبي

To a mixture of 7.0 g of 9-oxo-9,10-dihydro-4H-pyrrolo[1,2-a]thieno[2,3-e][1,4]diazepin in 25 ml of anhydrous tetrahydrofuran is added 9 ml of 10 molar boron-dimethylsulfide in tetrahydrofuran. The mixture is refluxed for 6 hours. The solution is cooled to room temperature and 25 ml of methanol added dropwise. The volatiles are removed under vacuum. To the residue is added 100 ml of 2N NaOH. The mixture is refluxed 5 hours and filtered. The solid is extracted with dichloromethane and the extract is washed with 2N citric acid, water and dried (Na2SO4). The solvent is removed in vacuo to give the desired product as a solid.

المصدر