Hydrochloric Acid → 1-(4-Hydroxy-3,5-di-isopropylphenyl)-2-p-tolyloxy-ethanone

HRID 1163464

반응식

HRID 1163464 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([O-:8])=[CH:4][CH:3]=1.[K+].Cl[CH2:11][C:12]([C:14]1[CH:19]=[C:18]([CH:20]([CH3:22])[CH3:21])[C:17]([OH:23])=[C:16]([CH:24]([CH3:26])[CH3:25])[CH:15]=1)=[O:13].Cl>CN(C)C=O>[OH:23][C:17]1[C:18]([CH:20]([CH3:22])[CH3:21])=[CH:19][C:14]([C:12](=[O:13])[CH2:11][O:8][C:5]2[CH:6]=[CH:7][C:2]([CH3:1])=[CH:3][CH:4]=2)=[CH:15][C:16]=1[CH:24]([CH3:26])[CH3:25]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 23676568Potassium 4-methylphenolateHCID 858900592-Chloro-1-(4-hydroxy-3,5-di-isopropylphenyl)-ethanone

생성물 1

HCID 577472281-(4-Hydroxy-3,5-di-isopropylphenyl)-2-p-tolyloxy-ethanone수율 36%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a solution of 4.47 g (30.6 mmol) of potassium 4-methylphenolate in 150 ml of dimethyl-formamide a solution of 3.90 g (15.3 mmol) of 2-chloro-1-(4-hydroxy-3,5-di-isopropylphenyl)-ethanone in 70 ml dimethylformamide is added at room temperature within a period of 100 minutes. After additional 2 hours of stirring at room temperature the pH is adjusted to 6-7 with 1 N HCl and the mixture is extracted with ethyl acetate. The collected organic phases are washed with water, dried and evaporated. Crystallization of the crude product from ethyl acetate/hexane gives 1.8 g of compound 105, m.p. 124-125° C.

후처리

  1. extractionthe mixture is extracted with ethyl acetate
  2. washThe collected organic phases are washed with water
  3. customdried
  4. customevaporated
  5. customCrystallization of the crude product from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-1397daaa6d5f4894b939af1dce66039d
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07820865B2

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