Toluene → HCID 57720058、化合物

HRID 1985593ノート

反応式

HRID 1985593 の反応式
[CH3:1][CH:2]([OH:7])[CH2:3][CH:4]([OH:6])[CH3:5].[C:8]1([CH3:18])[CH:13]=[CH:12][C:11](S(O)(=O)=O)=[CH:10][CH:9]=1.[C:19]1(C)C=CC=CC=1>>[CH3:5][CH:4]1[CH2:3][CH:2]([CH3:1])[O:7][C:9]2([CH:10]([CH3:19])[CH2:11][CH2:12][CH2:13][CH:8]2[CH3:18])[O:6]1

参加物

4

反応物 3

HCID 1140TolueneHCID 6101p-Toluenesulfonic acidHCID 122622,4-Pentanediol

生成物 1

HCID 57720058HCID 57720058、化合物

反応条件

温度
120 °C

実験手順

A reaction flask equipped with a Dean Stark trap was charged with 2,6-dimethyl cyclohehanone (252 g), 2,4-pentanediol (312 g), p-toluenesulfonic acid (6 g) and toluene (300 mL). The reaction mass was heated to reflux (110-130° C.). Water (36 mL) was collected in the Dean Stark trap. When no water was recovered, the reaction mass was cooled to an ambient temperature, neutralized with 10% aqueous sodium carbonate (100 mL) and washed with brine. Purification by vacuum distillation afforded 2,4,7,11-tetramethyl-1,5-dioxaspiro[5,5]undecane (339 g), which had a boiling point of 124° C. at a pressure of 40 mmHg.

後処理

  1. customA reaction flask equipped with a Dean Stark trap
  2. temperatureThe reaction mass was heated
  3. customWater (36 mL) was collected in the Dean Stark trap
  4. customWhen no water was recovered
  5. temperaturethe reaction mass was cooled to an ambient temperature
  6. washwashed with brine
  7. customPurification
  8. distillationby vacuum distillation

出典と根拠

ORDレコード
ord-fb988baafe3a43ea83de7719cdbf8854
出典データセット
uspto-grants-2009_06
特許番号
US07547668B1

反応ノート

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