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Hydrochloric Acid → Methyl alpha-methylthio-alpha-(m-benzoylphenyl)propionate

HRID 1660461
ノート
印刷プレビュー

反応式

HRID 1660461 の反応式
CO.[CH3:3][S:4][C:5]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17]2([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)OCC[O:18]2)[CH:12]=1)([CH3:10])[C:6]([O:8][CH3:9])=[O:7].Cl>O>[CH3:3][S:4][C:5]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17](=[O:18])[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:12]=1)([CH3:10])[C:6]([O:8][CH3:9])=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 12819455Methyl alpha-methylthio-alpha-[m-(2phenyl-1,3-dioxa-2-cyclopentyl)phenyl]propionate

生成物 1

HCID 13020172Methyl alpha-methylthio-alpha-(m-benzoylphenyl)propionate収率 95%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Methanol (10 ml) and 1 ml of water were added to 2.52 g of methyl α-methylthio-α-[m-(2-phenyl-1,3-dioxa-2-cyclopentyl)phenyl]propionate, and 0.2 ml of conc. hydrochloric acid was added. The mixture was heated for 20 minutes under reflux. After cooling, 20 ml of water was added, and the mixture was extracted with 50 ml and 10 ml respectively of methylene chloride. The extract was washed twice with 10 ml of water, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was chromatographed on a column of silica gel using methylene chloride as an eluent to afford 2.10 g of methyl α-methylthio-α-(m-benzoylphenyl)-propionate as a colorless oil in a yield of 95%.

後処理

  1. additionwas added
  2. temperatureThe mixture was heated for 20 minutes
  3. temperatureunder reflux
  4. temperatureAfter cooling
  5. extractionthe mixture was extracted with 50 ml and 10 ml respectively of methylene chloride
  6. washThe extract was washed twice with 10 ml of water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe solvent was evaporated under reduced pressure
  9. customThe residue was chromatographed on a column of silica gel

出典と根拠

ORDレコード
ord-c2898493bdba45d2a2fd105c3729f149
出典データセット
uspto-grants-1981_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04308208

反応ノート

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