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3-(3,4-Difluorophenyl)-2-methylprop-2-enoic acid → 3-(3,4-Difluorophenyl)-2-methylpropanoic acid

HRID 1954327
ノート
印刷プレビュー

反応式

HRID 1954327 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][C:13]=1[F:14])[CH:5]=[C:6]([CH3:10])[C:7]([OH:9])=[O:8]>CO.O=[Pt]=O>[F:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][C:13]=1[F:14])[CH2:5][CH:6]([CH3:10])[C:7]([OH:9])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 539805853-(3,4-Difluorophenyl)-2-methylprop-2-enoic acid

生成物 1

HCID 120521423-(3,4-Difluorophenyl)-2-methylpropanoic acid

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 887Methanol溶媒

実験手順

28 g (0.141 mol) of 3,4-difluoro-α-methylcinnamic acid, 1 g of PtO2 in 250 ml of MeOH is hydrogenated at 45 p.s.i. until the theoretical uptake is completed. The catalyst is filtered off, and the material evaporated to one-third its volume. A 15% potassium hydroxide solution (10 ml) is added, and the mixture refluxed for 30 minutes when it is poured into water and extracted with ether (2×100 ml). The aqueous layer is acidified with concentrated HCl and ice. The oil which comes out is extracted into ether, the ether solution dried over MgSO4 and evaporated to leave a clear oil which crystallizes. 3,4-difluoro-α-methylhydrocinnamic acid, M.P. 55-56° C., is isolated.

後処理

  1. filtrationThe catalyst is filtered off
  2. customthe material evaporated to one-third its volume
  3. additionA 15% potassium hydroxide solution (10 ml) is added
  4. temperaturethe mixture refluxed for 30 minutes when it
  5. additionis poured into water
  6. extractionextracted with ether (2×100 ml)
  7. extractionThe oil which comes out is extracted into ether
  8. dry with materialthe ether solution dried over MgSO4
  9. customevaporated
  10. customto leave a clear oil which
  11. customcrystallizes

出典と根拠

ORDレコード
ord-631131b4eeef4d68acac84872646ff65
出典データセット
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06121321

反応ノート

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