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

HRID 986033ノート

反応式

HRID 986033 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 136546961,2,2-Trichloro-3,3-dimethylcyclopropanecarboxylic acid収率 36.2%

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

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##

後処理

  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

出典と根拠

ORDレコード
ord-f02c2b3a76524b1fb639224867457987
出典データセット
uspto-grants-1987_12
特許番号
US04710518

反応ノート

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