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

HRID 36937ノート

反応式

HRID 36937 の反応式
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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-19b17b6c1f674e2c8896c8981d492d84
出典データセット
uspto-grants-1995_05
特許番号
US05418239

反応ノート

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