Sodium Hydroxide → Permethric acid

HRID 261459

반응식

HRID 261459 반응식
[Cl:1][C:2]([Cl:12])=[CH:3][C@@H:4]1[C@H:6]([C:7]([OH:9])=[O:8])[C:5]1([CH3:11])[CH3:10].[OH-].[Na+]>O>[Cl:1][C:2]([Cl:12])=[CH:3][CH:4]1[CH:6]([C:7]([OH:9])=[O:8])[C:5]1([CH3:10])[CH3:11]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 41507Cis-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane carboxylic acid2회

생성물 1

HCID 91658Permethric acid수율 87%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Conversion to high cis 3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropane-1-carboxylic acid (compound C acid). Sodium hydroxide (20 g, 0.5 mole) in 100 ml of water was added to the reaction mixture above with vigorous stirring and the whole was heated at 100° for 5 hours under conditions allowing for the distillation of the tert-butanol present from the Phase (a) reaction. The mixture was allowed to cool to room temperature, then washed with ether and made acidic with concentrated hydrochloric acid. The acidified mixture was extracted with ether and the ether extracts were combined, washed with brine, dried over magnesium sulfate and concentrated to give, after distillation, 18.22 g (87% yield) of 3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropane-1-carboxylic acid, bp 102°-105°/0.3 mm Hg, purity 97.3%, C/T=78/22.

후처리

  1. temperaturethe whole was heated at 100° for 5 hours under conditions
  2. distillationallowing for the distillation of the tert-butanol present from the Phase (a) reaction
  3. washwashed with ether
  4. extractionThe acidified mixture was extracted with ether
  5. washwashed with brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated
  8. customto give

출처 및 근거

ORD 기록
ord-7002097287ca43efa4a95f54092d8121
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04166064

연결된 노트

불러오는 중…