Cyclohexanone → Cyclohexanone, 2-(2-ethoxyethyl)-

HRID 2395856ノート

反応式

HRID 2395856 の反応式
[C:1]1(=[O:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(OOC(C)(C)C)(C)(C)C.[CH:18]([O:20][CH2:21][CH3:22])=[CH2:19]>>[CH2:18]([O:20][CH2:21][CH2:22][CH:2]1[CH2:3][CH2:4][CH2:5][CH2:6][C:1]1=[O:7])[CH3:19]

参加物

4

反応物 3

HCID 7967CyclohexanoneHCID 8023Ethyl vinyl etherHCID 8033Di-tert-butyl peroxide

生成物 1

HCID 11019297Cyclohexanone, 2-(2-ethoxyethyl)-収率 95%

実験手順

2940 g (30 mol) of cyclohexanone were heated to reflux while stirring and, at this temperature, a solution of 87.6 g (0.6 mol) of di-tert-butyl peroxide in 216 g (3 mol) of ethyl vinyl ether was added over the course of 5 hours (h). The mixture was subsequently refluxed for a further 1 h. After the mixture had cooled, the low boilers (tert-butanol, remaining vinyl ether and peroxide) and the excess cyclohexanone were removed by distillation under reduced pressure (25-40 mbar; diaphragm pump). The residue (about 500 g) was distilled under reduced pressure (0.5 to 2 mbar; oil pump). A total of 350 g of a 95% pure 2-(2-ethoxyethyl)cyclohexanone of boiling point 60°-65° C. (0.5 mbar) was obtained, corresponding to a yield of 69% of theory.

後処理

  1. temperatureto reflux
  2. temperatureThe mixture was subsequently refluxed for a further 1 h
  3. temperatureAfter the mixture had cooled
  4. customthe low boilers (tert-butanol, remaining vinyl ether and peroxide) and the excess cyclohexanone were removed by distillation under reduced pressure (25-40 mbar; diaphragm pump)
  5. distillationThe residue (about 500 g) was distilled under reduced pressure (0.5 to 2 mbar; oil pump)

出典と根拠

ORDレコード
ord-96ece210dd19420b8b8041f4b6f706f0
出典データセット
uspto-grants-1996_02
特許番号
US05489694

反応ノート

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