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Thionyl Chloride → Ethyl 2-(Chloromethyl)acrylate (stabilized with HQ)

HRID 1246221
ノート
印刷プレビュー

反応式

HRID 1246221 の反応式
S(Cl)([Cl:3])=O.O[CH2:6][C:7](=[CH2:13])[C:8]([O:10][CH2:11][CH3:12])=[O:9]>>[Cl:3][CH2:6][C:7](=[CH2:13])[C:8]([O:10][CH2:11][CH3:12])=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 24827Ethyl 2-(hydroxymethyl)-2-propenoate

生成物 1

HCID 11073578Ethyl 2-(Chloromethyl)acrylate (stabilized with HQ)収率 103.4%

実験手順

Thionyl chloride (10.6 g, 89.1 mmol) was dropwise added to ethyl α-hydroxymethylacrylate (10 g, 76.8 mmol) with ice-cooling; stirring was conducted for 30 minutes; then, a reaction was allowed to take place at 90° C. for 2 hours. After the completion of the reaction, low-boiling compounds were removed under reduced pressure to obtain unpurified ethyl α-chloromethylacrylate (11.8 g). Then, L-arabinoaminooxazoline (11.8 g, 64.0 mmol) was suspended in dimethylacetamide (80 ml). Thereto was dropwise added the ethyl α-chloromethylacrylate (11.8 g) with ice-cooling. A reaction was allowed to take place at room temperature for 4 hours. The reaction mixture was concentrated under reduced pressure to remove the solvent. To the residue was added isopropanol (100 ml), and the resulting mixture was stirred at room temperature for 1 hour. The resulting crystals were collected by filtration, washed with isopropanol (10 ml), and dried under reduced pressure to obtain a title compound (12.5 g g, 60.5%).

後処理

  1. temperaturecooling
  2. customat 90° C.
  3. customfor 2 hours
  4. customAfter the completion of the reaction, low-boiling compounds
  5. customwere removed under reduced pressure

出典と根拠

ORDレコード
ord-c9a88881df0a44578ed1c65fda92234f
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07125983B2

反応ノート

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