Pyridine → Cyclohexanone, 4-[(acetyloxy)methyl]-4-(4-chlorophenyl)-

HRID 1576217ノート

反応式

HRID 1576217 の反応式
[OH:1][CH2:2][C:3]1([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1.N1C=CC=CC=1.[C:23](OC(=O)C)(=[O:25])[CH3:24]>O>[C:23]([O:1][CH2:2][C:3]1([C:10]2[CH:11]=[CH:12][C:13]([Cl:16])=[CH:14][CH:15]=2)[CH2:4][CH2:5][C:6](=[O:9])[CH2:7][CH2:8]1)(=[O:25])[CH3:24]

参加物

5

反応物 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 215146584-(4-Chlorophenyl)-4-(hydroxymethyl)cyclohexan-1-one

生成物 1

HCID 12230249Cyclohexanone, 4-[(acetyloxy)methyl]-4-(4-chlorophenyl)-収率 66%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The 4-hydroxymethyl-4-(4-chlorophenyl)cyclohexanone is dissolved in 60 ml. of pyridine and 30 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, sodium bicarbonate solution and brine, and evaporated to dryness to give 12.8 g. (66% yield) of 4-acetoxymethyl-4-(4-chlorophenyl)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, sodium bicarbonate solution and brine
  4. customevaporated to dryness
  5. customto give 12.8 g

出典と根拠

ORDレコード
ord-cce86f7717ce486caf8f3b7c5480f6b1
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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