Water → 2,3,4,5-Tetrahydro-7-(phenylmethoxy)-1H-2-benzazepin-1-one

HRID 393564노트

반응식

HRID 393564 반응식
[C:1](=[O:4])([O-])[O-].[K+].[K+].[CH2:7](Br)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.[CH3:16][N:17](C)[CH:18]=[O:19]>>[CH2:7]([O:4][C:1]1[CH:11]=[CH:10][C:9]2[C:18](=[O:19])[NH:17][CH2:16][CH2:12][CH2:13][C:8]=2[CH:7]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

5

반응물 4

HCID 962WaterHCID 6228DimethylformamideHCID 7498Benzyl BromideHCID 11430Potassium Carbonate

생성물 1

HCID 222380502,3,4,5-Tetrahydro-7-(phenylmethoxy)-1H-2-benzazepin-1-one

실험 절차

Under atmosphere of argon, to a solution of the compound prepared in reference example 5 (4.79 g) in dimethylformamide (60 ml) were added potassium carbonate (11.2 g) and benzyl bromide (3.57 ml) at 0° C. and the mixture was stirred for 30 minutes at room temperature. To the reaction mixture was added water and was extracted with ethyl acetate. The organic layer was washed with water, a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride successively, and was dried over anhydrous magnesium sulfate and was concentrated. The residue was purified by column chromatography on silica gel (ethyl acetate:n-hexane=3:1) to give the title compound (3.8 g) having the following physical data.

후처리

  1. extractionwas extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materiala saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride successively, and was dried over anhydrous magnesium sulfate
  4. concentrationwas concentrated
  5. customThe residue was purified by column chromatography on silica gel (ethyl acetate:n-hexane=3:1)

출처 및 근거

ORD 기록
ord-19939fcb9cc949e7acd7e0bd7d6cf08b
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06809092B2

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