Sodium Hydroxide → 2-(2,5-Dichloro-4-methoxyphenyl)acetic acid

HRID 1930122

반응식

HRID 1930122 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([Cl:10])=[CH:4][C:3]=1[CH:11](C(OCC)=O)[C:12]([O:14]CC)=[O:13].[OH-].[Na+]>C1COCC1.CCO>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([Cl:10])=[CH:4][C:3]=1[CH2:11][C:12]([OH:14])=[O:13]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 59627728Diethyl 2-(2,5-dichloro-4-methoxyphenyl)malonate2회

생성물 1

HCID 52022252-(2,5-Dichloro-4-methoxyphenyl)acetic acid수율 60.7%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
60 °C

실험 절차

A solution of diethyl 2-(2,5-dichloro-4-methoxyphenyl)malonate (Intermediate 4-5; 1.88 g, 5.61 mmol) in THF (55 mL) and EtOH (5 mL) was treated with 2M sodium hydroxide (11.22 mL, 22.44 mmol) in one portion and the resulting solution was stirred at 60° C. for 17 hours. The reaction mixture was evaporated and the aqueous residue was acidified with 2M HCl. The precipitate was collected by filtration, washed with water (25 mL) and dried under vacuum to afford 2-(2,5-dichloro-4-methoxyphenyl)acetic acid (0.800 g, 60.7%) as a grey solid, which was used without further purification.

후처리

  1. customThe reaction mixture was evaporated
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water (25 mL)
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-1c6b304e486b48c9804a207ee40507f9
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188092B2

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