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2-(m-Nitrophenyl)-3,4-diazabicyclo[4.1.0]hept-2-en-5-one → HCID 23458522, 화합물

HRID 1679924
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반응식

HRID 1679924 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([C:10]2[CH:11]3[CH:13]([C:14](=[O:17])[NH:15][N:16]=2)[CH2:12]3)[CH:7]=[CH:8][CH:9]=1)([O-])=O>O1CCCC1.[Pd]>[NH2:1][C:4]1[CH:5]=[C:6]([C:10]2[CH:11]3[CH:13]([C:14](=[O:17])[NH:15][N:16]=2)[CH2:12]3)[CH:7]=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 234585112-(m-Nitrophenyl)-3,4-diazabicyclo[4.1.0]hept-2-en-5-one

생성물 1

HCID 23458522HCID 23458522, 화합물수율 69%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

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), dissolved in 80 ml of tetrahydrofuran, are hydrogenated with 0.5 g of 10% strength palladium on charcoal at room temperature. When the hydrogen absorption has ceased, the catalyst is filtered off and the filtrate is concentrated. The residue is recrystallized from an ethyl acetate/methanol mixture. 0.9 g (69% of theory) of 2-(m-aminophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one is obtained as colorless crystals, which are identical with the compound from Example 33.

후처리

  1. customWhen the hydrogen absorption
  2. filtrationthe catalyst is filtered off
  3. concentrationthe filtrate is concentrated
  4. customThe residue is recrystallized from an ethyl acetate/methanol mixture

출처 및 근거

ORD 기록
ord-5af43b8c4c4e406e9d64055ff8542ed9
출처 데이터셋
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04271163

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