Water → 1,2,2-Trichloro-3,3-dimethylcyclopropanecarboxylic acid

HRID 986033노트

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HRID 986033 반응식
[Cl:1][C:2]1([C:9]([O:11]C)=[O:10])[C:4]([CH3:6])([CH3:5])[C:3]1([Cl:8])[Cl:7].S(=O)(=O)(O)O.O>C(O)=O>[Cl:1][C:2]1([C:9]([OH:11])=[O:10])[C:4]([CH3:6])([CH3:5])[C:3]1([Cl:8])[Cl:7]

참가 물질

5

반응물 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 13654694Methyl 1,2,2-trichloro-3,3-dimethylcyclopropanecarboxylate

생성물 1

HCID 136546961,2,2-Trichloro-3,3-dimethylcyclopropanecarboxylic acid수율 36.2%

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

Methyl 1,2,2-trichloro-3,3-dimethylcyclopropanecarboxylate (10 g) was dissolved in formic acid (20 ml), and concentrated sulfuric acid (0.1 g) was added. The mixture was gently heated under reflux for 12 hours. After cooling, water (60 ml) was added to the reaction mixture. The precipitated crystals were collected by filtration, and recrystallized from hexane to give the desired 1,2,2-trichloro-3,3-dimethylcyclopropanecarboxylic acid (3.4 g) represented by the following formula. mp. 148°-150° C. ##STR25##

후처리

  1. temperatureThe mixture was gently heated
  2. temperatureunder reflux for 12 hours
  3. temperatureAfter cooling
  4. filtrationThe precipitated crystals were collected by filtration
  5. customrecrystallized from hexane

출처 및 근거

ORD 기록
ord-f02c2b3a76524b1fb639224867457987
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04710518

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