Cyclohexanone → Cyclohexanone

HRID 268192

反応式

HRID 268192 の反応式
[C:1]1(=[O:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.N[C:9]1([O:18]O)[CH2:14][CH:13]([CH3:15])[CH2:12][C:11]([CH3:17])([CH3:16])[CH2:10]1.S([O-])([O-])(=O)=O.[Mg+2]>S(=O)(=O)(O)O.C(O)C>[C:1]1(=[O:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:15][CH:13]1[CH2:12][C:11]([CH3:17])([CH3:16])[CH2:10][C:9](=[O:18])[CH2:14]1

参加物

7

反応物 3

HCID 7967CyclohexanoneHCID 24083Sulfuric acid magnesium salt (1:1)HCID 215101831-Amino-3,3,5-trimethylcyclohexyl hydroperoxide

生成物 2

HCID 7967CyclohexanoneHCID 133983,3,5-Trimethylcyclohexanone

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒HCID 702Ethanol溶媒

実験手順

To a stirred mixture of cyclohexanone (19.6 g.) and ethanol (50 c.c.), kept at or below 0°C, was added 1-amino-3,3,5-trimethylcyclohexyl hydroperoxide (17.3 g., 78% pure); solution was complete in ca. 10 min. To the solution was added conc. sulphuric acid (3 drops) and magnesium sulphate and the mixture was stored at 0°C for 3 days. The solid was filtered off, the filtrate washed with water, dried and distilled, to give cyclohexanone, dihydroisophorone and a fraction (11.5 g.), b.p. 90° - 100° at 0.02 mm.Hg., peroxide equivalent 179. By mass spectroscopy the product was shown to contain the unsymmetrical peroxide ##SPC32##

後処理

  1. custombelow 0°C
  2. waitthe mixture was stored at 0°C for 3 days
  3. filtrationThe solid was filtered off
  4. washthe filtrate washed with water
  5. customdried
  6. distillationdistilled

出典と根拠

ORDレコード
ord-59fda65d78fd4583bba70400ee0508f1
出典データセット
uspto-grants-1976_03
特許番号
US03947406

関連ノート

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