Acrylic Acid → 3-(2,3-Dichlorophenylthio)propanoic acid

HRID 865293

反応式

HRID 865293 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[SH:9].[C:10]([OH:14])(=[O:13])[CH:11]=[CH2:12].C([O-])([O-])=O.[Na+].[Na+]>>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[S:9][CH2:12][CH2:11][C:10]([OH:14])=[O:13]

参加物

4

反応物 3

HCID 6581Acrylic AcidHCID 10340Sodium CarbonateHCID 1402022,3-Dichlorobenzenethiol

生成物 1

HCID 218490133-(2,3-Dichlorophenylthio)propanoic acid収率 55.2%

反応条件

温度
50 °C

実験手順

2,3-Dichlorothiophenol (4.94 g, 28 mmol) was placed in a flask with acrylic acid (2.11 g, 29 mmol) and stirred at 50° C. for 3 hours. The reaction mixture was poured into 10% Na2CO3 and extracted with ether. The aqueous layer was acidified with concentrated hydrochloric acid, extracted with ether, washed with brine, dried over MgSO4, and concentrated in vacuo to give the 3-(2,3-dichlorophenylthio)propanoic acid (3.88 g), contaminated with some acrylic acid, as a clear oil which was used without further purification in the next step.

後処理

  1. extractionextracted with ether
  2. extractionextracted with ether
  3. washwashed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f663137862d0442db903ea1a97c05a71
出典データセット
uspto-grants-1996_10
特許番号
US05565482

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