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Triethylamine → 2,2-Dimethyl-1-(2-hydroxyethyl)-7-methoxy-3-(N-methyl-p-toluenesulphonamido)-1,2,3,4-tetrahydronaphthalene

HRID 65578
ノート
印刷プレビュー

反応式

HRID 65578 の反応式
[CH3:1][C:2]1([CH3:29])[CH:11]([N:12]([CH3:23])[S:13]([C:16]2[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=2)(=[O:15])=[O:14])[CH2:10][C:9]2[C:4](=[CH:5][C:6]([O:24][CH3:25])=[CH:7][CH:8]=2)[C:3]1=[CH:26][CH2:27][OH:28].C(N(CC)CC)C.[H][H]>CO.[Pd]>[CH3:1][C:2]1([CH3:29])[CH:11]([N:12]([CH3:23])[S:13]([C:16]2[CH:17]=[CH:18][C:19]([CH3:22])=[CH:20][CH:21]=2)(=[O:15])=[O:14])[CH2:10][C:9]2[C:4](=[CH:5][C:6]([O:24][CH3:25])=[CH:7][CH:8]=2)[CH:3]1[CH2:26][CH2:27][OH:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 54324160HCID 54324160、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 539916072,2-Dimethyl-1-(2-hydroxyethyl)-7-methoxy-3-(N-methyl-p-toluenesulphonamido)-1,2,3,4-tetrahydronaphthalene

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887
Methanol
溶媒

実験手順

2,2-Dimethyl-1-(2-hydroxyethylidene)-7-methoxy-3-(N-methyl-p-toluenesulphonamido)-1,2,3,4-tetrahydronaphthalene (15.5 g), dissolved in 250 ml of methanol, containing 2.2 ml of triethylamine, is submitted to catalytic hydrogenation, at atmosphere pressure and room temperature, the catalyst being 2.3 g 5% palladium on charcoal, The calculated amount of hydrogen is taken up within 1 hour. The catalyst is removed by filtration and the solvent by evaporation in vacuo. The residue is dissolved in chloroform and the solution is freed from basic material by means of washing with dilute hydrochloric acid and water, respectively. The dried solution is then concentrated in vacuo leaving a mixture containing two stereoisomers of the desired product. This mixture is suitable for further elaboration as described in example 13.

後処理

  1. customis submitted to catalytic hydrogenation, at atmosphere pressure and room temperature
  2. customThe catalyst is removed by filtration
  3. customthe solvent by evaporation in vacuo
  4. dissolutionThe residue is dissolved in chloroform
  5. washof washing with dilute hydrochloric acid and water
  6. concentrationThe dried solution is then concentrated in vacuo
  7. customleaving a mixture

出典と根拠

ORDレコード
ord-4b5c8432aa504bd78108d2880d9c6886
出典データセット
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04128548

反応ノート

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