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Ethylene Glycol → 2-Trityloxyethanol

HRID 80298
ノート
印刷プレビュー

反応式

HRID 80298 の反応式
[CH2:1]([OH:4])[CH2:2][OH:3].[C:5]1([C:11]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)Cl)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.O>N1C=CC=CC=1>[C:5]1([C:11]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)([C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[O:3][CH2:2][CH2:1][OH:4])[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 174Ethylene GlycolHCID 962WaterHCID 6456Trityl chloride

生成物 1

HCID 3167932-Trityloxyethanol収率 24%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
45 °C

実験手順

Ethylene glycol (3.10 g, 49.9 mmol) (Wako Pure Chemical Industries, Ltd.) and triphenylchloromethane (1.39 g, 49.9 mmol) (Wako Pure Chemical Industries, Ltd.) were dissolved in pyridine (6 mL) (Wako Pure Chemical Industries, Ltd.), and the solution was heated to 45° C. and stirred for 2 hours. Water (50 mL) was poured into the reaction solution, and mixture was extracted with toluene (Wako Pure Chemical Industries, Ltd.). The organic layer was dried with an hydrous sodium sulfate (Wako Pure Chemical Industries, Ltd.), and the solvent was distilled of funder reduced pressure. The residue was subjected to silica gel column chromatography (chloroform (Wako Pure Chemical Industries, Ltd.):methanol (Wako Pure Chemical Industries, Ltd.)=9:1), to thereby obtain the title compound (0.37 g, 24% yield).

後処理

  1. extractionwas extracted with toluene (Wako Pure Chemical Industries, Ltd.)
  2. dry with materialThe organic layer was dried with an hydrous sodium sulfate (Wako Pure Chemical Industries, Ltd.)
  3. distillationthe solvent was distilled of funder reduced pressure

出典と根拠

ORDレコード
ord-539387f15ac9479492f01f8763d5b64c
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846012B2

反応ノート

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