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

HRID 258044ノート

反応式

HRID 258044 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-0c84ae8e96fa4ed29b0756dcf506973d
出典データセット
uspto-grants-1993_11
特許番号
US05264454

反応ノート

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