4-(5-Bromo-2-methoxyphenyl)-4-methyl-2-oxopentanoic acid-ethyl ester → 4-(5-Bromo-2-methoxyphenyl)-4-methyl-2-oxopentanoic acid

HRID 2182650ノート

反応式

HRID 2182650 の反応式
C([O:3][C:4](=[O:20])[C:5](=[O:19])[CH2:6][C:7]([C:10]1[CH:15]=[C:14]([Br:16])[CH:13]=[CH:12][C:11]=1[O:17][CH3:18])([CH3:9])[CH3:8])C>CO.[OH-].[Na+]>[Br:16][C:14]1[CH:13]=[CH:12][C:11]([O:17][CH3:18])=[C:10]([C:7]([CH3:9])([CH3:8])[CH2:6][C:5](=[O:19])[C:4]([OH:20])=[O:3])[CH:15]=1

参加物

4

反応物 1

HCID 692032244-(5-Bromo-2-methoxyphenyl)-4-methyl-2-oxopentanoic acid-ethyl ester

生成物 1

HCID 219488674-(5-Bromo-2-methoxyphenyl)-4-methyl-2-oxopentanoic acid

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

4-(5-Bromo-2-methoxyphenyl)-4-methyl-2-oxopentanoic acid-ethyl ester in 30 ml of methanol and 12 ml of 1 M sodium hydroxide solution are stirred for 1 hour at room temperature, and the methanol is distilled off. It is mixed with water and hexane, the water phase is acidified with dilute hydrochloric acid while being cooled with ice, and it is mixed with ethyl acetate. The ethyl acetate phase is washed with water, dried (Na2SO4) and concentrated by evaporation. After crystallization from hexane, 1.8 g of 4-(5-bromo-2-methoxyphenyl)-4-methyl-2-oxopentanoic acid is obtained. Flash point: 80° C.

後処理

  1. distillationthe methanol is distilled off
  2. additionIt is mixed with water and hexane
  3. temperaturewhile being cooled with ice, and it
  4. additionis mixed with ethyl acetate
  5. washThe ethyl acetate phase is washed with water
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated by evaporation
  8. customAfter crystallization from hexane

出典と根拠

ORDレコード
ord-8dacb9070aba47c3b0d5b6b930a2d665
出典データセット
uspto-grants-2005_05
特許番号
US06897224B2

反応ノート

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