Lithium hydroxide, monohydrate → 4-(2-Methoxypropan-2-yl)benzoic acid

HRID 1479724

반응식

HRID 1479724 반응식
O.[OH-].[Li+].[CH3:4][O:5][C:6]([C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15]C)=[O:14])=[CH:11][CH:10]=1)([CH3:8])[CH3:7]>O1CCCC1.CO.O>[CH3:4][O:5][C:6]([C:9]1[CH:18]=[CH:17][C:12]([C:13]([OH:15])=[O:14])=[CH:11][CH:10]=1)([CH3:8])[CH3:7]

참가 물질

6

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 181744854-(1-Methoxy-1-methyl-ethyl)-benzoic acid methyl ester

생성물 1

HCID 181744324-(2-Methoxypropan-2-yl)benzoic acid수율 96.5%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Lithium hydroxide hydrate (0.40 g, 9.6 mmol) was added to a solution of methyl 4-(2-methoxypropan-2-yl)benzoate (0.10 g, 0.48 mmol) in tetrahydrofuran (9 mL), methanol (3 mL) and water (3 mL). The reaction mixture was stirred at room temperature for 2 hours. After the reaction, the solvent was removed in vacuo. Hydrochloric acid (3 mol/L) was added to make pH 2-3, and the product was extracted with dichloromethane (50 mL). The combined organic phase was washed with sodium chloride aqueous solution (50 mL×3), dried over anhydrous sodium sulfate, and the solvent was evaporated to dryness to give pure product 4-(2-methoxypropan-2-yl)benzoic acid (0.09 g, 96%) as a white solid.

후처리

  1. customAfter the reaction
  2. customthe solvent was removed in vacuo
  3. additionHydrochloric acid (3 mol/L) was added
  4. extractionthe product was extracted with dichloromethane (50 mL)
  5. washThe combined organic phase was washed with sodium chloride aqueous solution (50 mL×3)
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent was evaporated to dryness

출처 및 근거

ORD 기록
ord-5972453f5dc949d5aefa49f1c164e32b
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09409865B2

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