Water → Methyl 3,5-di-tert-butylbenzoate

HRID 37626노트

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HRID 37626 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH:11]=[C:12]([C:14]([CH3:17])([CH3:16])[CH3:15])[CH:13]=1)[C:8]([OH:10])=[O:9])([CH3:4])([CH3:3])[CH3:2].IC.[C:20](=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:2][C:1]([C:5]1[CH:6]=[C:7]([CH:11]=[C:12]([C:14]([CH3:17])([CH3:16])[CH3:15])[CH:13]=1)[C:8]([O:10][CH3:20])=[O:9])([CH3:4])[CH3:3]

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 853393,5-Bis(tert-butyl)benzoic acid

생성물 1

HCID 13267559Methyl 3,5-di-tert-butylbenzoate수율 97.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5.50 g (23.5 mmoles) of 3,5-di-t-butylbenzoic acid in 25 ml of dry dimethylformamide was added 5.01 g (35.3 mmoles) of iodomethane, and then 6.49 g of anhydrous potassium carbonate. After stirring at room temperature for 2 hours, water was added, the mixture was extracted three times with diethyl ether, the combined organic extracts were washed with brine, dried over sodium sulfate, filtered, and evaporated to give 5.68 g of the title compound as a crystalline solid, m.p. 52.0°-52.5° C. The structural assignment was supported by 1H NMR.

후처리

  1. extractionthe mixture was extracted three times with diethyl ether
  2. washthe combined organic extracts were washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-18c7bdf80cab41a8bc762755178fbc22
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420343

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