Propylene Glycol → 1,2-Propanediol ethyleneglycol monohydroxyoctadecyl ether

HRID 721997

反応式

HRID 721997 の反応式
[Cl-].[Ca+2].[Cl-].[O:4]1[CH:6]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH3:22])[CH2:5]1.S(=O)(=O)(O)O.[CH2:28]([OH:32])[CH:29]([OH:31])[CH3:30].O1C(CCCCCCCCCC)C1.C(=O)([O-])O.[Na+]>>[OH:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][O:31][CH2:29][CH2:28][OH:32].[CH2:28]([OH:32])[CH:29]([OH:31])[CH3:30]

参加物

7

反応条件

温度
72.5 °C

実験手順

Separately, a 1.0 liter mixing vessel equipped with a calcium chloride-containing tube was charged with 402.7 g (1.50 moles) of 1,2-epoxyoctadecane. While the charged 1,2-epoxyoctadecane was stirred at room temperature, a concentrated sulfuric acid was gradually dropped in an amount of 2.7 g (0.027 mole) into 1,2-epoxyoctadecane. After stirring for 15 minutes, the resultant mixture was placed into the dropping apparatus attached to the reaction vessel and was dropped into the 1,2-propanediol contained in the reaction vessel and maintained at a temperature of 70 to 75° C. over a time of 2 hours. Then the reaction of the mixture was carried out at a temperature of 70 to 75° C. for one hour. After the exhaustion of the starting material, namely 1,2-epoxydodecane was confirmed by a thin-layer chromatography, the reaction was stopped. A powdered sodium hydrogen carbonate was mixed in an amount of 2.5 g (0.03 mole) into the resultant reaction liquid in the reaction vessel, the resultant mixture was stirred for 30 minutes to neutralize the reaction liquid. From the reaction liquid, the precipitated crystals were separated by filtration. A 1,2-propanediol monohydroxyoctadecyl ether mixture was obtained in an amount of 510.9 g (yield: 96.7%).

後処理

  1. additionSeparately, a 1.0 liter mixing vessel
  2. additioncontaining tube
  3. customThen the reaction of the mixture
  4. waitwas carried out at a temperature of 70 to 75° C. for one hour
  5. customreaction liquid in the reaction vessel
  6. customthe reaction liquid
  7. customFrom the reaction liquid
  8. customthe precipitated crystals were separated by filtration

出典と根拠

ORDレコード
ord-82ca558d372e412aa7e838b3c0f07146
出典データセット
uspto-grants-2006_11
特許番号
US07138365B2

関連ノート

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