Potassium Hydroxide → 2-[4-(8-Hydroxy-2,2,4,4-tetramethyl-chroman-6-ylethynyl)-phenyl]-2-methyl-propionic acid

HRID 1869861노트

반응식

HRID 1869861 반응식
C[O:2][C:3](=[O:30])[C:4]([C:7]1[CH:12]=[CH:11][C:10]([C:13]#[C:14][C:15]2[CH:16]=[C:17]3[C:22](=[C:23]([OH:25])[CH:24]=2)[O:21][C:20]([CH3:27])([CH3:26])[CH2:19][C:18]3([CH3:29])[CH3:28])=[CH:9][CH:8]=1)([CH3:6])[CH3:5].[OH-].[K+]>CO.O1CCCC1>[OH:25][C:23]1[CH:24]=[C:15]([C:14]#[C:13][C:10]2[CH:11]=[CH:12][C:7]([C:4]([CH3:6])([CH3:5])[C:3]([OH:30])=[O:2])=[CH:8][CH:9]=2)[CH:16]=[C:17]2[C:22]=1[O:21][C:20]([CH3:27])([CH3:26])[CH2:19][C:18]2([CH3:29])[CH3:28]

참가 물질

5

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온도
80 °C

실험 절차

A solution of 2-[4-(8-hydroxy-2,2,4,4-tetramethyl-chroman-6-ylethynyl)-phenyl]-2-methyl-propionic acid methyl ester (Intermediate 23, 0.035 g, 0.087 mmol) in methanol (2 mL) and tetrahydrofuran (1 mL) was treated with a 1M solution of potassium hydroxide (2 mL, 4 mmol) and the resulting reaction mixture was stirred at 80° C. for 2 h. The volatiles were evaporated in vacuo to a residue that was neutralized with saturated aqueous ammonium chloride solution and extracted with ethyl acetate. The organic phase was washed with water and brine, and dried over anhydrous magnesium sulfate, filtered and evaporated in vacuo to afford the title product as a yellow solid (0.034 g, 100%).

후처리

  1. customthe resulting reaction mixture
  2. customThe volatiles were evaporated in vacuo to a residue that
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was washed with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-e01de9489e624fe09892bb68dc491ed8
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07638648B2

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