반응 #83533

반응 방정식

iso-valeryl chloride

10,11-dihydro-10-(4-amino-3-methoxybenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

triethylamine

→

residue

수율 129.1%

10,11-Dihydro-10-[4-[(3-methylbutanoyl)amino]benzoyl]-5H-pyrrolo[2,1-c][1,4]benzodiazepine

수율 129.1%

용매

methylene chloride

반응 조건

후처리

1. 1
   기타quenched with 1N NaOH
2. 2
   기타The organic layer is evaporated in vacuo to a residue which
3. 3
   workup.STIRRINGis stirred in 5 ml of tetrahydrofuran for 1 hour
4. 4
   기타evaporated in vacuo to a residue
5. 5
   추출The residue is extracted with ethyl acetate-methylene chloride
6. 6
   세척washed with brine
7. 7
   건조dried (Na2SO4)
8. 8
   여과filtered through hydrous magnesium silicate
9. 9
   기타evaporated in vacuo

실험 절차

To a stirred solution of 0.10 g of 10,11-dihydro-10-(4-amino-3-methoxybenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 1 ml of methylene chloride is added 0.06 g of triethylamine followed by 0.05 g of iso-valeryl chloride. The reaction mixture is stirred for 3 hours and then quenched with 1N NaOH. The organic layer is evaporated in vacuo to a residue which is stirred in 5 ml of tetrahydrofuran for 1 hour, then evaporated in vacuo to a residue. The residue is extracted with ethyl acetate-methylene chloride, washed with brine, dried (Na2SO4), filtered through hydrous magnesium silicate and evaporated in vacuo to give 0.15 g of residue which is stirred with ether-hexane to give 0.13 g of light yellow solid. MS(CI): 418(M+H).

출처