반응 #3638

반응 방정식

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

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   온도The mixture is refluxed for 6 hours
2. 2
   기타The volatiles are removed under vacuum
3. 3
   workup.ADDITIONTo the residue is added 100 ml of 2N NaOH
4. 4
   온도The mixture is refluxed 5 hours
5. 5
   여과filtered
6. 6
   추출The solid is extracted with dichloromethane
7. 7
   세척the extract is washed with 2N citric acid, water
8. 8
   건조dried (Na2SO4)
9. 9
   기타The solvent is removed in vacuo

실험 절차

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.

출처