Benzene → 2-Cyclohexen-1-one, 2,6,6-trimethyl-3-(2-methylpropoxy)-

HRID 1974214ノート

反応式

HRID 1974214 の反応式
[CH3:1][CH:2]1[C:7](=[O:8])[CH:6]=[CH:5][C:4]([CH3:10])([CH3:9])[C:3]1=[O:11].C1C=CC=CC=1.[CH2:18](O)[CH:19]([CH3:21])[CH3:20].CC1C=CC(S(O)(=O)=O)=CC=1>O>[CH3:1][C:2]1[C:3](=[O:11])[C:4]([CH3:10])([CH3:9])[CH2:5][CH2:6][C:7]=1[O:8][CH2:18][CH:19]([CH3:21])[CH3:20]

参加物

6

反応物 4

HCID 241BenzeneHCID 6101p-Toluenesulfonic acidHCID 6560IsobutanolHCID 70585111HCID 70585111、化合物

生成物 1

HCID 109217652-Cyclohexen-1-one, 2,6,6-trimethyl-3-(2-methylpropoxy)-

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The compound 2,6,6-trimethylcyclohexen-1,3-dione (43.6 g) was added to a mixture of benzene (250 ml), isobutanol (50 ml) and PTSA (500 mg) and heated under reflux for 3 hr in conjunction with a Dean and Stark water separator. The reaction was then cooled to room temperature, washed with aqueous sodium carbonate solution and brine and taken to dryness "in vacuo". Distillation of residue through a 6 inch vacuum jacketed vigreaux column yielded pure 2,6,6-trimethyl-3-isobutoxycyclohex-2-en-1 one (54.6 g) bp 104°-107°.

後処理

  1. temperatureheated
  2. washwashed with aqueous sodium carbonate solution and brine
  3. distillationDistillation of residue through a 6 inch vacuum

出典と根拠

ORDレコード
ord-7e5a5b28ea4845dda657d116fed47b92
出典データセット
uspto-grants-1976_12
特許番号
US04000198

反応ノート

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