Acetone → 3,4-Dimethoxy-6-(2-bromoisonicotinoyl)benzaldehyde

HRID 1739423노트

반응식

HRID 1739423 반응식
C[O:2][CH:3](OC)[C:4]1[C:9]([C:10](=[O:18])[C:11]2[CH:16]=[CH:15][N:14]=[C:13]([Br:17])[CH:12]=2)=[CH:8][C:7]([O:19][CH3:20])=[C:6]([O:21][CH3:22])[CH:5]=1.Cl.CC(C)=O>O>[CH3:22][O:21][C:6]1[CH:5]=[C:4]([C:9]([C:10](=[O:18])[C:11]2[CH:16]=[CH:15][N:14]=[C:13]([Br:17])[CH:12]=2)=[CH:8][C:7]=1[O:19][CH3:20])[CH:3]=[O:2]

참가 물질

5

반응물 3

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 218408043,4-Dimethoxy-6-(2-bromoisonicotinoyl)benzaldehyde dimethyl acetal

생성물 1

HCID 218408403,4-Dimethoxy-6-(2-bromoisonicotinoyl)benzaldehyde수율 70.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

3,4-Dimethoxy-6-(2-bromoisonicotinoyl)benzaldehyde dimethyl acetal (13.9 g) and 2 M hydrochloric acid (1 ml) are added to a mixture of acetone (30 ml) and water (5 ml), and the mixture is stirred at room temperature for two hours. The mixture is evaporated to remove the acetone, and the remaining aqueous layer is extracted with chloroform. The extract is washed, dried, and concentrated. The residue is purified by silica gel column chromatography (solvent; chloroform:ethyl acetate=4:1) to give 3,4-dimethoxy-6-(2-bromoisonicotinoyl)benzaldehyde (8.65 g).

후처리

  1. customThe mixture is evaporated
  2. customto remove the acetone
  3. extractionthe remaining aqueous layer is extracted with chloroform
  4. washThe extract is washed
  5. customdried
  6. concentrationconcentrated
  7. customThe residue is purified by silica gel column chromatography (solvent; chloroform:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-d71b43967f4e4db4a96ba6b9f56f5a72
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05965730

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