Dimethylformamide → 3,4,5-Trichlorothiophene-2-carbonyl chloride

HRID 1870496

反応式

HRID 1870496 の反応式
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([Cl:8])[S:4][C:3]=1[C:9]([OH:11])=O.S(Cl)([Cl:14])=O.CN(C=O)C>ClCCCl>[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([Cl:8])[S:4][C:3]=1[C:9]([Cl:14])=[O:11]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 41685843,4,5-Trichloro-2-thiophenecarboxylic acid

生成物 1

HCID 70103083,4,5-Trichlorothiophene-2-carbonyl chloride

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A mixture of 20.4 g (0.088 mole) of 3,4,5-trichloro-2-thiophenecarboxylic acid, 7.3 mL (0.1 mole) of thionyl chloride, 0.2 mL of DMF and 80 mL of 1,2-dichloroethane was heated at reflux temperature for 3 h. The reaction mixture became a clear solution after 1 h of heating. The mixture was allowed to cool to RT, concentrated in vacuo and exposed to high vacuum to give 22.0 g (>98% wt) an oil which solidified upon standing to an off-white powder, mp 37°-41° C.

後処理

  1. temperaturewas heated
  2. temperatureat reflux temperature for 3 h
  3. customafter 1 h
  4. temperatureof heating
  5. concentrationconcentrated in vacuo
  6. customto give 22.0 g (>98% wt) an oil which

出典と根拠

ORDレコード
ord-3a0e30aa59a6439f901066c5650f5030
出典データセット
uspto-grants-2000_08
特許番号
US06096898

関連ノート

読み込み中…