Water → 2-(4-Fluorophenyl)-2-methylbutanoic acid

HRID 1589456ノート

反応式

HRID 1589456 の反応式
[CH2:1]([C:3]([C:12]#N)([CH3:11])[C:4]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][CH:5]=1)[CH3:2].S(=O)(=O)(O)[OH:15].[OH2:19]>>[F:10][C:7]1[CH:8]=[CH:9][C:4]([C:3]([CH3:11])([CH2:1][CH3:2])[C:12]([OH:15])=[O:19])=[CH:5][CH:6]=1

参加物

4

反応物 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 13199826alpha-Ethyl-alpha-methyl-4-fluorobenzyl cyanide

生成物 1

HCID 137117812-(4-Fluorophenyl)-2-methylbutanoic acid

実験手順

7.6 g of crude α-ethyl-α-methyl-4-fluorobenzyl cyanide, 20 ml of H2O and 20 ml of concentrated sulfuric acid were refluxed at 134° to 137° C. for 5.5 hours. The mixture was cooled to room temperature and extracted with benzene, and the benzene solution was extracted with dilute alkali and the obtained dilute alkali extract was adjusted to pH 7.5 with concentrated hydrochloric acid, and extracted with benzene to remove impurities. Then, the aqueous solution was adjusted to pH 4.6 with concentrated hydrochloric acid and extracted with benzene. The benzene extract was washed with water, dried over Na2SO4, and evaporated under reduced pressure to give 3.8 g of 2-(4-fluorophenyl)-2-methylbutyric acid.

後処理

  1. extractionextracted with benzene
  2. extractionthe benzene solution was extracted with dilute alkali
  3. additionthe obtained dilute alkali
  4. extractionextract
  5. extractionextracted with benzene
  6. customto remove impurities
  7. extractionextracted with benzene
  8. extractionThe benzene extract
  9. washwas washed with water
  10. dry with materialdried over Na2SO4
  11. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-54463866957047b083e2336fc6f53999
出典データセット
uspto-grants-1986_02
特許番号
US04570005

反応ノート

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