Trifluoroacetic acid → 2,4-Difluoro-3-vinylbenzoic acid

HRID 658096노트

반응식

HRID 658096 반응식
FC(F)(F)C(O)=O.[F:8][C:9]1[C:21]([CH:22]=[CH2:23])=[C:20]([F:24])[CH:19]=[CH:18][C:10]=1[C:11]([O:13]C(C)(C)C)=[O:12]>ClCCl>[F:8][C:9]1[C:21]([CH:22]=[CH2:23])=[C:20]([F:24])[CH:19]=[CH:18][C:10]=1[C:11]([OH:13])=[O:12]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 68451303Tert-butyl 2,4-difluoro-3-vinylbenzoate

생성물 1

HCID 684536492,4-Difluoro-3-vinylbenzoic acid수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A 4.27 ml portion of trifluoroacetic acid was added to 30 ml of dichloromethane solution containing 1.33 g of tert-butyl 2,4-difluoro-3-vinylbenzoate and stirred for 5 hours. After evaporation of the solvent, appropriate amounts of purified water and saturated sodium bicarbonate aqueous solution were added thereto and the water layer was washed with diethyl ether. The water layer was adjusted to pH 1 with 1 M hydrochloric acid aqueous solution, extracted with diethyl ether and then dried with anhydrous magnesium sulfate. After concentration, 964 mg (95%) of 2,4-difluoro-3-vinylbenzoic acid (Reference Example 6-1) was obtained.

후처리

  1. customAfter evaporation of the solvent, appropriate amounts of purified water and saturated sodium bicarbonate aqueous solution
  2. additionwere added
  3. washthe water layer was washed with diethyl ether
  4. extractionextracted with diethyl ether
  5. dry with materialdried with anhydrous magnesium sulfate
  6. concentrationAfter concentration

출처 및 근거

ORD 기록
ord-dee5542b17c24c0abc972d8d95cbaa24
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076367B2

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