Triethylamine → HCID 18917528, 화합물

HRID 1290943

반응식

HRID 1290943 반응식
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[CH:21]=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:4][CH:3]=1.[CH3:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[CH2:31][C:32](Cl)=[O:33].C(N(CC)CC)C>ClCCl>[CH:23]1[CH:22]=[CH:21][N:13]2[CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[N:10]([C:8]([C:5]3[CH:4]=[CH:3][C:2]([NH:1][C:32](=[O:33])[CH2:31][C:26]4[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=4[CH3:24])=[N:7][CH:6]=3)=[O:9])[CH2:11][C:12]=12

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 2760632o-Tolyl-acetyl chlorideHCID 1891750110, 11-dihydro-10-(6-amino-3-pyridinylcarbonyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

생성물 1

HCID 18917528HCID 18917528, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 2.0 mmol of 10,11-dihydro-10-(6-amino-3-pyridinylcarbonyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 2.1 mmol of 2-methylbenzeneacetyl chloride and 5 mmol of triethylamine in 10 ml of dichloromethane is stirred under argon at room temperature for 16 hours. The solvent is removed under vacuum and the residue partitioned between 50 ml of ethyl acetate and 25 ml of water. The organic layer is separated, washed with H2O, 1N NaHCO3, brine and dried (Na2SO4). The solvent is removed and the residue chromatographed on silica gel with ethyl acetate-hexane as solvent to give the product as a solid.

후처리

  1. customThe solvent is removed under vacuum
  2. customthe residue partitioned between 50 ml of ethyl acetate and 25 ml of water
  3. customThe organic layer is separated
  4. washwashed with H2O, 1N NaHCO3, brine
  5. dry with materialdried (Na2SO4)
  6. customThe solvent is removed
  7. customthe residue chromatographed on silica gel with ethyl acetate-hexane as solvent

출처 및 근거

ORD 기록
ord-78c2d3ccbabc42dbb5d01c81da310956
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753648

연결된 노트

불러오는 중…