Pentaerythritol → Karenz MT

HRID 2061298ノート

反応式

HRID 2061298 の反応式
[OH:1][CH2:2][C:3]([CH2:8][OH:9])([CH2:6][OH:7])[CH2:4][OH:5].[SH:10][CH:11]([CH3:16])[CH2:12][C:13]([OH:15])=O.[OH2:17].C1(C)[CH:23]=[CH:22][C:21]([S:24](O)(=O)=O)=[CH:20]C=1>C1(C)C=CC=CC=1>[SH:24][CH:21]([CH3:20])[CH2:22][C:23]([O:1][CH2:2][C:3]([CH2:8][O:9][C:13](=[O:15])[CH2:12][CH:11]([SH:10])[CH3:16])([CH2:6][O:7][C:13](=[O:15])[CH2:12][CH:11]([SH:10])[CH3:16])[CH2:4][O:5][C:13](=[O:15])[CH2:12][CH:11]([SH:10])[CH3:16])=[O:17]

参加物

5

反応物 3

HCID 8285PentaerythritolHCID 521998p-Toluenesulfonic acid monohydrateHCID 99640843-Mercaptobutyric acid

生成物 1

HCID 54576326Karenz MT

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
140 °C

実験手順

In a 300 ml egg plant type flask, 26 g (102 mmol) of pentaerythritol (available from Tokyo Chemical Industry, Co., Ltd.), 54 g (450 mmol) of 3-mercaptobutanoic acid (available from Yodo Chemical Co., Ltd.), 2.6 g (13.5 mmol) of p-toluenesulfonic acid monohydrate (available from Junsei Chemical Co., Ltd.) and 100 g of toluene (available from Junsei Chemical Co., Ltd.) were placed, and a Dean-Stark device and a cooling tube were installed. The contents in the flask were heated at an oil bath temperature of 140° C. with stirring. After 4 hours from the initiation of reaction, the reaction solution was allowed to cool, washed with ion-exchanged water and then neutralized with a saturated sodium hydrogencarbonate aqueous solution. The resulting solution was further washed with ion-exchanged water three times and then subjected to dehydration-drying using anhydrous magnesium sulfate (available from Junsei Chemical Co., Ltd.). Next, toluene was distilled off, and the remainder was subjected to column chromatography by a silica gel to perform purification of PEMB. As the silica gel, Wako Gel C-200 (available from Wako Pure Chemical Industries, Ltd.) was used, and as the elution solvent, n-hexane/acetone (7/1 by volume) was used. The PEMB obtained by purification was a colorless transparent liquid, and the yield was 24.5 g (21%).

後処理

  1. customAfter 4 hours from the initiation of reaction
  2. temperatureto cool
  3. washwashed with ion-exchanged water
  4. washThe resulting solution was further washed with ion-exchanged water three times
  5. customto dehydration-drying
  6. distillationNext, toluene was distilled off
  7. custompurification of PEMB

出典と根拠

ORDレコード
ord-97b3d5fa68724bffa9a43511f8d461b1
出典データセット
uspto-grants-2012_10
特許番号
US08283095B2

反応ノート

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