Sulfuryl chloride → Ethyl 2-chloro-3-oxo-4-phenylbutyrate

HRID 1173779

反応式

HRID 1173779 の反応式
[O:1]=[C:2]([CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].S(Cl)([Cl:19])(=O)=O>C(Cl)Cl>[Cl:19][CH:3]([C:2](=[O:1])[CH2:9][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)[C:4]([O:6][CH2:7][CH3:8])=[O:5]

参加物

4

反応物 2

HCID 24648Sulfuryl chlorideHCID 225855Ethyl 3-oxo-4-phenylbutanoate

生成物 1

HCID 11601176Ethyl 2-chloro-3-oxo-4-phenylbutyrate収率 86.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
20 °C

実験手順

Ethyl 3-oxo-4-phenylbutyrate (4.8 g, 23 mmol) and methylene chloride (48 ml) were mixed, and sulfuryl chloride (3.1 g, 1 equivalent) was gradually added thereto dropwise. After the addition, the mixture was stirred at 20° C. for 1 hour. The reaction mixture was concentrated under reduced pressure, and saturated aqueous solution of sodium hydrogencarbonate (10 ml) was added, and extraction was carried out with ethyl acetate (20 ml). The solvent was evaporated away under reduced pressure and drying was carried out in vacuum to obtain the title compound as a yellow oil (4.8 g, yield: 86%).

後処理

  1. additionAfter the addition
  2. concentrationThe reaction mixture was concentrated under reduced pressure, and saturated aqueous solution of sodium hydrogencarbonate (10 ml)
  3. additionwas added
  4. extractionextraction
  5. customThe solvent was evaporated away under reduced pressure
  6. customdrying

出典と根拠

ORDレコード
ord-e6baa6b5b8594ff7abbfbb4adeb29779
出典データセット
uspto-grants-2010_11
特許番号
US07834190B2

関連ノート

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