Pyridine → [1-(3,4-Dimethoxyphenyl)-4-oxocyclohexyl]methyl acetate

HRID 1576220ノート

反応式

HRID 1576220 の反応式
[OH:1][CH2:2][C:3]1([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([O:18][CH3:19])[CH:11]=2)[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1.N1C=CC=CC=1.[C:26](OC(=O)C)(=[O:28])[CH3:27]>O>[C:26]([O:1][CH2:2][C:3]1([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([O:18][CH3:19])[CH:11]=2)[CH2:4][CH2:5][C:6](=[O:9])[CH2:7][CH2:8]1)(=[O:28])[CH3:27]

参加物

5

反応物 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 215146714-(3,4-Dimethoxyphenyl)-4-(hydroxymethyl)cyclohexan-1-one

生成物 1

HCID 21514706[1-(3,4-Dimethoxyphenyl)-4-oxocyclohexyl]methyl acetate収率 57%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The 4-hydroxymethyl-4-(3,4-dimethoxyphenyl)cyclohexanone is dissolved in 20 ml. of pyridine and 10 ml. of acetic anhydride. After about 20 hours of standing at room temperature, the mixture is poured into ice and water. The gum that precipitates is extracted with ether. The organic layer is washed successively with water, 2.5 N hydrochloric acid, water and brine, and evaporated to dryness to give 6.43 g. (57% yield) of 4-acetoxymethyl-4-(3,4-dimethoxyphenyl)cyclohexanone, as an amorphous gum.

後処理

  1. customThe gum that precipitates
  2. extractionis extracted with ether
  3. washThe organic layer is washed successively with water, 2.5 N hydrochloric acid, water and brine
  4. customevaporated to dryness
  5. customto give 6.43 g

出典と根拠

ORDレコード
ord-4393d21c72bb42839169441d1910a593
出典データセット
uspto-grants-1976_09
特許番号
US03979444

反応ノート

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