4-Hydroxybenzaldehyde → 4-[(1-Trityl-4-imidazolyl)methoxy]benzaldehyde

HRID 53994

반응식

HRID 53994 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.Cl[CH2:11][C:12]1[N:13]=[CH:14][N:15]([C:17]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:16]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[C:17]([N:15]1[CH:16]=[C:12]([CH2:11][O:1][C:2]2[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=2)[N:13]=[CH:14]1)([C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1)([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

참가 물질

5

반응물 3

HCID 1264-HydroxybenzaldehydeHCID 11430Potassium CarbonateHCID 27631764-(Chloromethyl)-1-trityl-1H-imidazole

생성물 1

HCID 154290374-[(1-Trityl-4-imidazolyl)methoxy]benzaldehyde수율 51.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.22 g of p-hydroxybenzaldehyde and 4.08 g of 4-chloromethyl-1-tritylimidazole were dissolved in 40 ml of N,N-dimethylformamide, followed by adding 1.66 g of anhydrous potassium carbonate and subsequently stirring at room temperature for 40 hours. The thus prepared reaction solution were partitioned between water and benzene, and the resulting organic layer was concentrated to dryness. The resulting residue was purified by subjecting it to silica gel column chromatography using chloroform as an elution solvent, and the thus purified product was crystallized from a n-hexane/benzene solvent system. In this way, 2.3 g of the title compound was obtained.

후처리

  1. customThe thus prepared reaction solution
  2. customwere partitioned between water and benzene
  3. concentrationthe resulting organic layer was concentrated to dryness
  4. customThe resulting residue was purified
  5. customthe thus purified product was crystallized from a n-hexane/benzene solvent system

출처 및 근거

ORD 기록
ord-17eb8a45e2594e19a819e59a7d8dfe7b
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05620991

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