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对甲苯磺酰氯 → HCID 11076628,化合物

HRID 1753685
笔记
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反应方程式

HRID 1753685 反应方程式
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.C1COCC1.[CH3:17][O:18][CH2:19][CH2:20][O:21][CH2:22][CH2:23][OH:24].[OH-].[Na+]>O>[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7]([O:24][CH2:23][CH2:22][O:21][CH2:20][CH2:19][O:18][CH3:17])(=[O:9])=[O:8])=[CH:3][CH:2]=1
参与物实验过程后处理来源与证据反应笔记

参与物

6

反应物 4

HCID 7397对甲苯磺酰氯HCID 8028四氢呋喃2 次HCID 8134二乙二醇单甲醚HCID 14798氢氧化钠

产物 1

HCID 11076628HCID 11076628,化合物收率 101.7%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

Under ice cooling, a mixture of 515 g of p-toluenesulfonyl chloride and 500 ml of THF was added dropwise to a mixture of 295 g of 2-(2-methoxyethoxy)ethanol, 589 g of 25 wt % NaOH aqueous solution, and 2,500 ml of THF. The reaction solution was aged for 1.5 hours, after which 1,500 ml of water was added to quench the reaction. The organic layer was separated and concentrated in vacuum. The concentrate was dissolved in a mixture of 660 ml toluene and 330 ml hexane, and washed with water. The organic layer was concentrated in vacuum, obtaining 684.74 g of the target compound, 2-(2-methoxyethoxy)ethyl p-toluenesulfonate as oily matter. Yield 97%.

后处理

  1. customto quench
  2. customthe reaction
  3. customThe organic layer was separated
  4. concentrationconcentrated in vacuum
  5. dissolutionThe concentrate was dissolved in a mixture of 660 ml toluene and 330 ml hexane
  6. washwashed with water
  7. concentrationThe organic layer was concentrated in vacuum

来源与证据

ORD记录
ord-2036542604194db1a90de657546d519e
来源数据集
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
专利号
US09164384B2

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记