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

HRID 658096ノート

反応式

HRID 658096 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 684536492,4-Difluoro-3-vinylbenzoic acid収率 95%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dee5542b17c24c0abc972d8d95cbaa24
出典データセット
uspto-grants-2011_12
特許番号
US08076367B2

反応ノート

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