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

HRID 1163464

反応式

HRID 1163464 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1397daaa6d5f4894b939af1dce66039d
出典データセット
uspto-grants-2010_10
特許番号
US07820865B2

関連ノート

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