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2-Chlorobenzaldehyde → HCID 21276949, 화합물

HRID 2292138
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HRID 2292138 반응식
[C:1]([NH:5][C:6](=[O:11])/[CH:7]=[C:8](\[NH2:10])/[CH3:9])([CH3:4])([CH3:3])[CH3:2].[Cl:12][C:13]1[CH:20]=[CH:19][CH:18]=[CH:17][C:14]=1[CH:15]=O.[CH3:21][N:22]1[C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=2[N:24]=[C:23]1[CH2:31][CH2:32][CH2:33][O:34][CH2:35][C:36](=O)[CH2:37][C:38]([O:40][CH2:41][CH3:42])=[O:39]>C(O)C>[C:1]([NH:5][C:6]([C:7]1[CH:15]([C:14]2[CH:17]=[CH:18][CH:19]=[CH:20][C:13]=2[Cl:12])[C:37]([C:38]([O:40][CH2:41][CH3:42])=[O:39])=[C:36]([CH2:35][O:34][CH2:33][CH2:32][CH2:31][C:23]2[N:22]([CH3:21])[C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=3[N:24]=2)[NH:10][C:8]=1[CH3:9])=[O:11])([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 69962-ChlorobenzaldehydeHCID 19864533HCID 19864533, 화합물HCID 21276958HCID 21276958, 화합물

생성물 1

HCID 21276949HCID 21276949, 화합물수율 14.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

N-t-Butyl-3-aminocrotonamide (0.63 g), 2-chlorobenzaldehyde (0.56 g) and ethyl 4-[3-(1-methylbenzimidazol-2-yl)propoxy]-3-ketobutanoate (1.27 g) were dissolved in ethanol (16 ml) and stirred under reflux for 15 hours. The reaction mixture was cooled and the solvent removed under reduced pressure. The residue was chromatographed on silica eluting with 3% methanol in ethyl acetate. The fractions containing the product were combined and evaporated. Recrystallisation of the resulting foam from ethanol yielded the title compound as a white solid (0.33 g, 14%), m.p. 202° C. Found: C, 66.17; H, 6.92; N, 9.48. C32H39ClN4O4 requires C, 66.36; H, 6.79; N, 9.68%.

후처리

  1. temperatureunder reflux for 15 hours
  2. temperatureThe reaction mixture was cooled
  3. customthe solvent removed under reduced pressure
  4. customThe residue was chromatographed on silica eluting with 3% methanol in ethyl acetate
  5. additionThe fractions containing the product
  6. customevaporated
  7. customRecrystallisation of the resulting foam from ethanol

출처 및 근거

ORD 기록
ord-c27ae321195640029b193d16ba75816b
출처 데이터셋
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04801598

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