Sodium Acetate → 3-(2-Methylbenzoyl)-5,6,7,8-tetrahydro-2-naphthol

HRID 36937노트

반응식

HRID 36937 반응식
Br[C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[CH:5]=[C:4]([C:12](=[O:20])[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[CH3:19])[C:3]=1[OH:21].C([O-])(=O)C.[Na+]>[Pd].CO>[CH3:19][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=1[C:12]([C:4]1[C:3]([OH:21])=[CH:2][C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[CH:5]=1)=[O:20]

참가 물질

5

반응물 2

HCID 517045Sodium AcetateHCID 100204261-Bromo-3-(2-methylbenzoyl)-5,6,7,8-tetrahydro-2-naphthol

생성물 1

HCID 103782473-(2-Methylbenzoyl)-5,6,7,8-tetrahydro-2-naphthol수율 96.5%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of 1-bromo-3-(2-methylbenzoyl)-5,6,7,8-tetrahydro-2-naphthol (3.33 g), sodium acetate (0.82 g), 5% palladium-on-carbon (50% hydrate, 1.0 g) and methanol (10 ml) was subjected to catalytic reduction. After the theoretical amount of hydrogen had been absorbed, the catalyst was filtered off. The solvent was then distilled off and the residue was diluted with water and extracted with ethyl acetate. The extract was washed with water and dried (MgSO4) and the solvent was distilled off to give 3-(2-methylbenzoyl)-5,6,7,8-tetrahydro-2-naphthol as an oil (2.45 g, 96.5%).

후처리

  1. customAfter the theoretical amount of hydrogen had been absorbed
  2. filtrationthe catalyst was filtered off
  3. distillationThe solvent was then distilled off
  4. additionthe residue was diluted with water
  5. extractionextracted with ethyl acetate
  6. washThe extract was washed with water
  7. dry with materialdried (MgSO4)
  8. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-19b17b6c1f674e2c8896c8981d492d84
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05418239

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