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

HRID 2054933노트

반응식

HRID 2054933 반응식
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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 14798Sodium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-266b4f04dcee458b82113b082262a062
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07329753B2

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