Potassium Carbonate → 3-(Dimethylamino)methyl-1,2,3,4-tetrahydro-7-quinolinol

HRID 382964노트

반응식

HRID 382964 반응식
C(=O)([O-])[O-].[K+].[K+].Cl.Cl.[CH3:9][N:10]([CH2:12][CH:13]1[CH2:22][C:21]2[C:16](=[CH:17][C:18]([O:23]C)=[CH:19][CH:20]=2)[NH:15][CH2:14]1)[CH3:11]>>[CH3:11][N:10]([CH2:12][CH:13]1[CH2:22][C:21]2[C:16](=[CH:17][C:18]([OH:23])=[CH:19][CH:20]=2)[NH:15][CH2:14]1)[CH3:9]

참가 물질

3

반응물 2

HCID 11430Potassium CarbonateHCID 229986093-(N,N-dimethylamino)methyl-1,2,3,4-tetrahydro-7-methoxyquinoline dihydrochloride

생성물 1

HCID 219397443-(Dimethylamino)methyl-1,2,3,4-tetrahydro-7-quinolinol수율 115.1%

실험 절차

A solution of 3-(N,N-dimethylamino)methyl-1,2,3,4-tetrahydro-7-methoxyquinoline dihydrochloride (1.0 g) 48% hydrobromic acid (10 ml) was heated under reflux for 4 hr. The reaction mixture was poured into 10% aqueous potassium carbonate and extracted with ethyl acetate. The organic layer was dried and concentrated. The resulting crude crystals were recrystallized from ethyl acetate-hexane to obtain the titled compound (0.81 g). The melting point of its dihydrochloride was 151-152° C. (recrystallizing solvent; methanol-diisopropyl ether).

후처리

  1. temperatureunder reflux for 4 hr
  2. extractionextracted with ethyl acetate
  3. customThe organic layer was dried
  4. concentrationconcentrated
  5. customThe resulting crude crystals were recrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-a5507607c2a947929e1d9e49e79512ad
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06310107B1

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