Pyridine → trans-3-[2-Chloro-3,3,3-trifluoropropenyl]-2,2-dimethylcyclopropanecarbonyl chloride

HRID 444244노트

반응식

HRID 444244 반응식
[Cl:1][C:2]([C:12]([F:15])([F:14])[F:13])=[CH:3][C@H:4]1[C@H:6]([C:7](O)=[O:8])[C:5]1([CH3:11])[CH3:10].N1C=CC=CC=1.S(Cl)([Cl:24])=O>C1(C)C=CC=CC=1>[Cl:1][C:2]([C:12]([F:15])([F:14])[F:13])=[CH:3][C@H:4]1[C@H:6]([C:7]([Cl:24])=[O:8])[C:5]1([CH3:11])[CH3:10]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 86736787trans-3-[2-Chloro-3,3,3-trifluoropropenyl]-2,2-dimethylcyclopropanecarboxylic acid

생성물 1

HCID 86736786trans-3-[2-Chloro-3,3,3-trifluoropropenyl]-2,2-dimethylcyclopropanecarbonyl chloride수율 84.1%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a stirred solution of 4.1 g (0.0173 mole) of trans-3-(2-chloro-3,3,3-trifluoro-1-propenyl)-2,2-dimethylcyclopropanecarboxylic acid in 40 ml of toluene at ambient temperature was added 1.7 g (0.022 mole) of pyridine, then 2.6 g (0.022 mole) of thionyl chloride in 25 ml of toluene. Upon complete addition the reaction mixture was stirred at ambient temperature for 17 hours. The reaction mixture was filtered through diatomaceous earth, and the filtrate was evaporated under reduced pressure to give 3.8 g of trans-3-(2-chloro-3,3,3-trifluoro-1-propenyl)-2,2-dimethylcyclopropanecarbonyl chloride. The ir spectrum was consistent with the assigned structure.

후처리

  1. additionUpon complete addition the reaction mixture
  2. filtrationThe reaction mixture was filtered through diatomaceous earth
  3. customthe filtrate was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-65eadc139cee4f878740467f6c037710
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04263319

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