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Triethylamine → 5,6-Dihydro-6-(4-nitrobenzoyl)-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine

HRID 3559
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HRID 3559 반응식
[CH:1]1[N:5]2[C:6]3[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=3[NH:8][CH2:9][CH2:10][C:4]2=[N:3][N:2]=1.C(N(CC)CC)C.[N+:22]([C:25]1[CH:33]=[CH:32][C:28]([C:29](Cl)=[O:30])=[CH:27][CH:26]=1)([O-:24])=[O:23]>ClCCl>[N+:22]([C:25]1[CH:26]=[CH:27][C:28]([C:29]([N:8]2[C:7]3[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=3[N:5]3[CH:1]=[N:2][N:3]=[C:4]3[CH2:10][CH2:9]2)=[O:30])=[CH:32][CH:33]=1)([O-:24])=[O:23]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 85024-Nitrobenzoyl chlorideHCID 218370045,6-Dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine

생성물 1

HCID 218372105,6-Dihydro-6-(4-nitrobenzoyl)-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a mixture of 3 mmol of 5,6-dihydro-4H-[1,2,4]-triazolo[4,3-a][1,5]benzodiazepine in 10 ml of dichloromethane under argon is added 5 mmol of triethylamine. To the mixture is added dropwise 3.3 mmol of 4-nitrobenzoyl chloride in 3 ml of dichloromethane. The mixture is stirred at room temperature 3 hours and then washed with water, aqueous NaHCO3 and brine. The organic layer is dried (Na2SO4) and the solvent removed under vacuum. The residue is purified by chromatography on silica gel to give the desired product as a solid.

후처리

  1. washwashed with water, aqueous NaHCO3 and brine
  2. dry with materialThe organic layer is dried (Na2SO4)
  3. customthe solvent removed under vacuum
  4. customThe residue is purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-51928d820704485fb5ee2dc349f44abc
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05733905

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