Water → HCID 86740262、化合物

HRID 485506

反応式

HRID 485506 の反応式
[CH3:1][C:2]([CH3:7])([CH2:5][OH:6])[CH:3]=[O:4].[CH2:8]([C:10]([CH2:15][OH:16])([CH2:13][OH:14])[CH2:11][CH3:12])[OH:9].C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1C=CC=CC=1.C1CCCCC1>[CH3:1][C:2]([CH3:7])([CH2:5][OH:6])[CH:3]=[O:4].[CH2:8]([C:10]([CH2:15][OH:16])([CH2:13][OH:14])[CH2:11][CH3:12])[OH:9]

参加物

7

反応物 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 6510TrimethylolpropaneHCID 116993-Hydroxy-2,2-dimethylpropionaldehyde

生成物 1

HCID 86740262HCID 86740262、化合物

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回HCID 8078Cyclohexane溶媒2 回

実験手順

250 parts of 2,2-dimethyl-3-hydroxypropanal, 328 parts of trimethylolpropane, 16.4 parts of p-toluenesulfonic acid, 520 parts of benzene and 130 parts of cyclohexane were charged in a 2-1 reactor provided with a stirrer, thermostat, thermometer, condenser and separator. The mixture was heated. Water formed was distilled together with the solvent and condensed. Water alone was taken out of the system by means of the separator and the solvent was returned into the reactor. When 44 parts of water was formed, the reaction system was cooled. The reaction temperature was 70° to 85° C. The reaction mixture was dissolved in 2400 parts of benzene and 600 parts of cyclohexane and washed with 500 parts of a 20% aqueous common salt solution three times. The solvents were distilled off under reduced pressure to obtain 2,2-dimethyl-3-hydroxypropanal/trimethylolpropane condensate. The condensate was a white solid having a hydroxyl value of 515.1 and a melting point of 119° to 120.8° C.

後処理

  1. customprovided with a stirrer
  2. temperatureThe mixture was heated
  3. distillationwas distilled together with the solvent and condensed
  4. customWhen 44 parts of water was formed
  5. temperaturethe reaction system was cooled
  6. customwas 70° to 85° C
  7. washwashed with 500 parts of a 20% aqueous common salt solution three times
  8. distillationThe solvents were distilled off under reduced pressure

出典と根拠

ORDレコード
ord-e7e30b1a0218464087177eb92ad41389
出典データセット
uspto-grants-1985_08
特許番号
US04536588

関連ノート

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