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HCID 54184183、化合物 → HCID 53931433、化合物

HRID 261539
ノート
印刷プレビュー

反応式

HRID 261539 の反応式
[CH3:1][O:2][C:3](=[O:19])[C:4](=O)[C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][C:13]=1[Cl:14])[CH2:10][C:9]([CH2:16][CH3:17])([CH3:15])[CH2:8]2.[H][H]>CO.S(=O)(=O)(O)O.[Pt](=O)=O>[CH3:1][O:2][C:3](=[O:19])[CH2:4][C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][C:13]=1[Cl:14])[CH2:10][C:9]([CH2:16][CH3:17])([CH3:15])[CH2:8]2
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 2

HCID 54184183HCID 54184183、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 53931433HCID 53931433、化合物

試薬・触媒・溶媒 3

HCID 345198Adams' catalyst触媒HCID 887Methanol溶媒HCID 1118Sulfuric Acid溶媒

実験手順

A solution of 5.2 g of 2-ethyl-6-chloro-2-methyl-α-oxo-5-indanacetic acid methyl ester in 100 cc of methanol and 10 cc of concentrated sulphuric acid is hydrogenated at 45° and a hydrogen pressure of 5 atmospheres with the addition of 1.0 g of platinum(IV) oxide. After the take up of the theoretic amount of hydrogen the catalyst is filtered off, the solution is diluted with a 5% sodium bicarbonate solution and extracted with ether. The extract is washed with water, dried over sodium sulphate and concentrated by evaporation. The resulting title compound is purified by chromatography. Thin layer chromatogram: Rf value 0.60 (adsorbent: silica gel, eluant: chloroform).

後処理

  1. customis hydrogenated at 45°
  2. filtrationAfter the take up of the theoretic amount of hydrogen the catalyst is filtered off
  3. additionthe solution is diluted with a 5% sodium bicarbonate solution
  4. extractionextracted with ether
  5. washThe extract is washed with water
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated by evaporation
  8. customThe resulting title compound is purified by chromatography

出典と根拠

ORDレコード
ord-3c680a05fcd44f4d8351be645d3fcffd
出典データセット
uspto-grants-1979_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04166131

反応ノート

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