Catechol → 2-(2,2,2-Trifluoroethyl)-2-(trifluoromethyl)-1,3-benzodioxole

HRID 1081290노트

반응식

HRID 1081290 반응식
[C:1]1([C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4])[OH:2].Cl[C:10](=[CH:15][C:16]([F:19])([F:18])[F:17])[C:11]([F:14])([F:13])[F:12]>[OH-].[Na+]>[F:12][C:11]([F:14])([F:13])[CH2:10][C:15]1([C:16]([F:19])([F:18])[F:17])[O:4][C:3]2[CH:5]=[CH:6][CH:7]=[CH:8][C:1]=2[O:2]1

참가 물질

4

반응물 2

HCID 289CatecholHCID 98152-Chloro-1,1,1,4,4,4-hexafluoro-2-butene

생성물 1

HCID 536673032-(2,2,2-Trifluoroethyl)-2-(trifluoromethyl)-1,3-benzodioxole

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

11 g of pyrocatechol were dissolved in 200 ml of dimethylfomamide, and 18 g of 45% strength by weight aqueous sodium hydroxide solution were added. 20 g of 2-chloro-1,1,1,4,4,4-hexafluoro-2-butene were added dropwise at 75° C. to the mixture. Stirring was continued for 30 minutes at 75° C. The mixture was then poured into 500 ml of ice-water and extracted with diethyl ether. The organic phase was washed with water, dried with magnesium sulphate and concentrated. Finally, the product was distilled under a high vacuum. The yield was 15 g (=56%) the boiling point was 60° C. at 10 mbar. The NMR spectra showed the following characteristic absorptions: 19F-NMR: -59.0 and -84.6 ppm; 1H-NMR: 3.02 ppm.

후처리

  1. additionwere added
  2. extractionextracted with diethyl ether
  3. washThe organic phase was washed with water
  4. dry with materialdried with magnesium sulphate
  5. concentrationconcentrated
  6. distillationFinally, the product was distilled under a high vacuum

출처 및 근거

ORD 기록
ord-8a6dd1e3092f43ad88674ab6fe02bd53
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05585395

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