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Hydrazine hydrate (1:1) → HCID 11405060, 화합물

HRID 2421833
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HRID 2421833 반응식
[C:1]([N:4]1[C:10]([CH3:11])=[CH:9][C:8]2[CH:12]=[CH:13][C:14]([Cl:16])=[CH:15][C:7]=2[C:6]([C:17]2[CH:22]=[CH:21][C:20]([N+:23]([O-])=O)=[C:19]([CH3:26])[CH:18]=2)=[N:5]1)(=[O:3])[CH3:2].O.NN>CO.ClCCl.[Ni]>[C:1]([N:4]1[C:10]([CH3:11])=[CH:9][C:8]2[CH:12]=[CH:13][C:14]([Cl:16])=[CH:15][C:7]=2[C:6]([C:17]2[CH:22]=[CH:21][C:20]([NH2:23])=[C:19]([CH3:26])[CH:18]=2)=[N:5]1)(=[O:3])[CH3:2]
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참가 물질

6

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 11428649HCID 11428649, 화합물

생성물 1

HCID 11405060HCID 11405060, 화합물수율 79%

시약·촉매·용매 3

HCID 935Nickel촉매HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

0.78 g (2.1 mmoles) of 3-acetyl-8-chloro-4-methyl-1-(3-methyl-4-nitrophenyl)-3H-2,3-benzodiazepine are dissolved in the mixture of 15 ml of methanol and 15 ml of dichloromethane, and about 0.5 g of wet Raney-nickel catalyst and 0.26 ml (5.25 mmoles) of 98% hydrazine hydrate are subsequently added to it under vigorous stirring. The mixture is stirred for further 1 hour. The catalyst is filtered off, washed with dichloromethane, the filtrate is evaporated and the residue is solidified by rubbing with 15 ml of water. The crude product is recrystallized from ethanol. Thus 0.56 g (79%) of the desired compound melting at 209-211° C. is obtained.

후처리

  1. additionare subsequently added to it under vigorous stirring
  2. filtrationThe catalyst is filtered off
  3. washwashed with dichloromethane
  4. customthe filtrate is evaporated
  5. customThe crude product is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-705999548eaa4a278e0894c535941e4d
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07960375B2

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