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

HRID 1870496

반응식

HRID 1870496 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3a0e30aa59a6439f901066c5650f5030
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06096898

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