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Hydrazine hydrate (1:1) → HCID 23458522, 화합물

HRID 1679925
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HRID 1679925 반응식
O.NN.[N+:4]([C:7]1[CH:8]=[C:9]([C:13]2[CH:14]3[CH:16]([C:17](=[O:20])[NH:18][N:19]=2)[CH2:15]3)[CH:10]=[CH:11][CH:12]=1)([O-])=O>C(O)C.[Ni]>[NH2:4][C:7]1[CH:8]=[C:9]([C:13]2[CH:14]3[CH:16]([C:17](=[O:20])[NH:18][N:19]=2)[CH2:15]3)[CH:10]=[CH:11][CH:12]=1
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참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 234585112-(m-Nitrophenyl)-3,4-diazabicyclo[4.1.0]hept-2-en-5-one

생성물 1

HCID 23458522HCID 23458522, 화합물수율 76.5%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매2회

실험 절차

A solution of 0.65 g (13.0 millimoles) of hydrazine hydrate in 10 ml of ethanol is added, whilst stirring, to a mixture of 1.5 g (6.5 millimoles) of 2-(m-nitrophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one (see Example 32b), 20 ml of ethanol and a small amount of an aqueous Raney nickel suspension in the course of 5 minutes, during which the temperature rises from 25° to 35° C. Stirring is continued for 1 hour and the reaction mixture is then slowly raised to the boil. It is refluxed for 5 minutes and filtered hot, and the filtrate is concentrated. After recrystallization from ethyl acetate/methanol, 1.0 g (76% of theory) of 2-(m-aminophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one is obtained as colorless crystals, identical with the compound from Example 33.

후처리

  1. customin the course of 5 minutes
  2. customrises from 25° to 35° C
  3. temperaturethe reaction mixture is then slowly raised to the boil
  4. temperatureIt is refluxed for 5 minutes
  5. filtrationfiltered hot
  6. concentrationthe filtrate is concentrated
  7. customAfter recrystallization from ethyl acetate/methanol

출처 및 근거

ORD 기록
ord-76815d093611414aaacc6057aa4facfb
출처 데이터셋
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04271163

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