2,3-Butanediol → HCID 57720059、化合物

HRID 1985590ノート

反応式

HRID 1985590 の反応式
[CH3:1][CH:2]([OH:6])[CH:3]([OH:5])[CH3:4].[C:7]1([CH3:17])[CH:12]=[CH:11][C:10](S(O)(=O)=O)=[CH:9][CH:8]=1.[C:18]1(C)C=CC=CC=1>>[CH3:4][CH:3]1[CH:2]([CH3:1])[O:6][C:8]2([CH:9]([CH3:18])[CH2:10][CH2:11][CH2:12][CH:7]2[CH3:17])[O:5]1

参加物

4

反応物 3

HCID 2622,3-ButanediolHCID 1140TolueneHCID 6101p-Toluenesulfonic acid

生成物 1

HCID 57720059HCID 57720059、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 (200 g), 2,3-butanediol (315 g), p-toluenesulfonic acid (2 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 2,3,6,10-tetramethyl-1,4-dioxaspiro[4,5]decane (265 g)), which had a boiling point of 104° C. at a pressure of 16 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 the reaction mass
  5. temperaturewas 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-23dfa52ab24445c69b979b71f0097541
出典データセット
uspto-grants-2009_06
特許番号
US07547667B1

反応ノート

読み込み中…