Sulfuryl chloride → Ethyl 2-chloro-3-cyclopropyl-3-oxopropanoate

HRID 2275774ノート

反応式

HRID 2275774 の反応式
S(Cl)([Cl:4])(=O)=O.[CH:6]1([C:9](=[O:16])[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH2:8][CH2:7]1>ClCCl>[Cl:4][CH:10]([C:9]([CH:6]1[CH2:8][CH2:7]1)=[O:16])[C:11]([O:13][CH2:14][CH3:15])=[O:12]

参加物

4

反応物 2

HCID 24648Sulfuryl chlorideHCID 262979Ethyl 3-cyclopropyl-3-oxopropanoate

生成物 1

HCID 54244501Ethyl 2-chloro-3-cyclopropyl-3-oxopropanoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3.1 ml of sulphuryl chloride (38.2 mmol, 1.05 equivalents) were initially charged in 21 ml of dichloromethane, and 5.68 g of ethyl 3-cyclopropyl-3-oxopropanoate (36.4 mmol) were added dropwise on a water bath. The reaction mixture was stirred at RT for 2 h. The mixture was then washed with water, 5% strength aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution, dried over magnesium sulphate and concentrated. The crude product (6.8 g) was used without further purification for the next reaction.

後処理

  1. washThe mixture was then washed with water, 5% strength aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution
  2. dry with materialdried over magnesium sulphate
  3. concentrationconcentrated
  4. customThe crude product (6.8 g) was used without further purification for the next reaction

出典と根拠

ORDレコード
ord-91476b64f3a6405788f68526136596eb
出典データセット
uspto-grants-2015_09
特許番号
US09126998B2

反応ノート

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