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4-Toluenesulfonyl chloride → HCID 11076628, 화합물

HRID 1753685
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HRID 1753685 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 73974-Toluenesulfonyl chlorideHCID 8028Tetrahydrofuran2회HCID 8134Diethylene Glycol Monomethyl EtherHCID 14798Sodium Hydroxide

생성물 1

HCID 11076628HCID 11076628, 화합물수율 101.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-2036542604194db1a90de657546d519e
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09164384B2

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