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1-Butanol → Butan-1-ol;2-ethyl-2-(hydroxymethyl)propane-1,3-diol;titanium

HRID 247050
ノート
印刷プレビュー

反応式

HRID 247050 の反応式
CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4:17].[CH2:18]([C:20]([CH2:25][OH:26])([CH2:23][OH:24])[CH2:21][CH3:22])[OH:19].[CH2:27]([OH:45])[CH2:28][CH2:29][CH2:30]CCCCCCCCCCCCCC.C(O)CCC>>[CH2:18]([C:20]([CH2:25][OH:26])([CH2:23][OH:24])[CH2:21][CH3:22])[OH:19].[CH2:27]([OH:45])[CH2:28][CH2:29][CH3:30].[Ti:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 2631-ButanolHCID 6510TrimethylolpropaneHCID 8221Stearyl AlcoholHCID 11026Titanium isopropoxide

生成物 1

HCID 22960090Butan-1-ol;2-ethyl-2-(hydroxymethyl)propane-1,3-diol;titanium

実験手順

A liquid mixture of 28.4 g (0.1 mole) of tetraisopropyl titanate, 4.5 g (0.033 mole) of trimethylolpropane, 0.1 g (0.0004 mole) of stearyl alcohol and an excess amount, i.e., 100 g (1.37 moles) of butanol was heated under reflux to dissolve the solid substance completely. The resultant isopropyl alcohol and butanol were then distilled off to obtain trimethylolpropane-butyl alcohol-titanate (polyol titanate). The polyol titanate was then cooled by ice, followed by an addition of butanol which contained 1.8002 g (0.10 mole) of water. After heating the resultant mixture to form a uniform solution, butanol was removed by distillation. Under cooling, butanol with 0.9005 g (0.05 mole) of water incorporated therein was added again. The resultant mixture was heated to effect polymerization and crosslinking. Butanol was then removed thoroughly under reduced pressure. After heating the residue again at 100° C. for 30 minutes in water-containing butanol, the product was dried under reduced pressure to obtain 12.2 g of a solid substance. This solid substance had such properties that it showed water repellency when water was added thereto but its surface was wet immediately when an alcohol was added thereto.

後処理

  1. temperatureunder reflux
  2. dissolutionto dissolve the solid substance completely
  3. distillationThe resultant isopropyl alcohol and butanol were then distilled off

出典と根拠

ORDレコード
ord-4fe6e30855704a1a97963f93d14fa807
出典データセット
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04705764

反応ノート

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