Phenol → Carbonic acid, butyl phenyl ester

HRID 565081

反応式

HRID 565081 の反応式
[C:1](=[O:12])([O:7][CH2:8][CH2:9][CH2:10][CH3:11])[O:2][CH2:3][CH2:4][CH2:5][CH3:6].[C:13]1(O)C=CC=C[CH:14]=1.C(=O)(OCCCC)N>[O-]CCCC.[O-]CCCC.[O-]CCCC.[O-]CCCC.[Ti+4]>[C:1](=[O:12])([O:2][C:3]1[CH:14]=[CH:13][CH:6]=[CH:5][CH:4]=1)[O:7][CH2:8][CH2:9][CH2:10][CH3:11]

参加物

5

反応物 3

HCID 996PhenolHCID 11596n-Butyl carbamateHCID 68333Dibutyl carbonate

生成物 1

HCID 564930Carbonic acid, butyl phenyl ester収率 12.3%

試薬・触媒・溶媒 1

HCID 21801Titanium tetrabutoxide触媒

実験手順

1795 g of the top section liquid obtained above containing 862 g of dibutyl carbonate, 932 g of phenol and 1 g of butyl carbamate and 16.8 g of titanium tetrabutoxide were charged into a round bottom flask of capacity 5 L in which a distillation column made from glass provided with a vacuum jacket (filled Sulzer Labopacking, inner diameter 50mmφ, height of filling portion 1100 mm) was connected to an upper portion thereof. The contents in the flask were heated with a mantle heater while stirring at 300 rpm with a mechanical stirrer. When the bottom section temperature became 191° C., reflux was started. All reflux was performed for 10 minutes after starting of reflux and then distillation-out was started in a reflux ratio of 30. The starting time of distillation-out was regarded as starting of the reaction. The yield (mol %) of butyl phenyl carbonate based on charged dibutyl carbonate was analyzed by gas chromatography. The yield was 12.3% in the reaction for 30 min., 18.6% in the reaction for 60 min., 22.5% in the reaction for 90 min., 27.4% in the reaction for 120 min., and 30.0% in the reaction for 150 min. The amount of distilled-out liquid was 131 g and the distilled-out liquid contained 128 g of butanol and 3 g of phenol. The bottom section temperature was 192° C. at the starting time of distillation-out and 197° C. after 150 minutes of starting of the reaction.

後処理

  1. custom1795 g of the top section liquid obtained
  2. additionwere charged into a round bottom flask of capacity 5 L in which
  3. distillationa distillation column
  4. customprovided with a vacuum jacket (filled Sulzer Labopacking, inner diameter 50mmφ, height of filling portion 1100 mm)
  5. temperatureThe contents in the flask were heated with a mantle heater
  6. custombecame 191° C.
  7. temperaturereflux
  8. temperatureof reflux
  9. distillationdistillation-out
  10. distillationThe starting time of distillation-out
  11. customas starting of the reaction

出典と根拠

ORDレコード
ord-bf560b23e3614318b4284930546dbc86
出典データセット
uspto-grants-2001_01
特許番号
US06169197A

関連ノート

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