3-(2,4-Dichlorophenyl)propanoic acid → 4,6-Dichloro-1-indanone

HRID 430070

反応式

HRID 430070 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][CH2:10][C:11]([OH:13])=O>O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]2[C:3]=1[CH2:9][CH2:10][C:11]2=[O:13]

参加物

3

反応物 1

HCID 27409153-(2,4-Dichlorophenyl)propanoic acid

生成物 1

HCID 122065184,6-Dichloro-1-indanone収率 4.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

3-(2,4-dichlorophenyl)propanoic acid (0.44 g, 2 mmol) in polyphosphoric acid (7 g) was heated to 100° C. under argon. After 90 min the mixture was cooled and treated with water (20 ml) and extracted with hexane (40 ml). The hexane layer was dried (MgSO4), and evaporated to dryness. The residue was purified by column chromatography on silica gel eluting with 0-30% dichloromethane in hexane to give the title product as a yellow solid, (0.018 g, 4.5%), δH (CDCl3) 2.8 (2H, m), 3.1 (2H, m), 7.6 (1H, d), 7.65 (1H, d).

後処理

  1. temperatureAfter 90 min the mixture was cooled
  2. extractionextracted with hexane (40 ml)
  3. dry with materialThe hexane layer was dried (MgSO4)
  4. customevaporated to dryness
  5. customThe residue was purified by column chromatography on silica gel eluting with 0-30% dichloromethane in hexane

出典と根拠

ORDレコード
ord-bdaed1af101f4a3fb37531108d241fdc
出典データセット
uspto-grants-2001_11
特許番号
US06320051B1

関連ノート

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