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Dimethylformamide → HCID 117666794, 화합물

HRID 1753681
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HRID 1753681 반응식
[C:1]1([S:7][C:8]2[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:15][O:16][CH2:17][CH2:18]Cl.C(=O)([O-])[O-].[K+].[K+].CN(C=O)C>C1(C)C=CC=CC=1.O>[C:1]1([S:7][C:8]2[CH:13]=[CH:12][C:11]([O:14][CH2:18][CH2:17][O:16][CH3:15])=[CH:10][CH:9]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 123162-Chloroethyl methyl etherHCID 113101954-(phenylthio)phenol

생성물 1

HCID 117666794HCID 117666794, 화합물수율 101%

시약·촉매·용매 2

HCID 962Water용매
HCID 1140
Toluene
용매

실험 절차

A solution was prepared by combining 10 g of 4-hydroxyphenyl phenyl sulfide which had been synthesized according to the well-known formulation, 5 g of 2-chloroethyl methyl ether, 7.4 g of potassium carbonate, and 20 g of DMF. The solution was aged at 80° C. for 16 hours. The aged solution was cooled to room temperature, to which 20 g of water was added to quench the reaction. To the solution, 40 g of toluene was added for extraction. The organic layer was separated and washed with sodium hydroxide aqueous solution and water in sequence. The organic layer was concentrated in vacuum, obtaining 13 g of the target compound, 4-(2-methoxyethoxy)phenyl phenyl sulfide as oily matter. Yield 93%.

후처리

  1. customA solution was prepared
  2. customhad been synthesized
  3. additionwas added
  4. customto quench
  5. customthe reaction
  6. customThe organic layer was separated
  7. washwashed with sodium hydroxide aqueous solution and water in sequence
  8. concentrationThe organic layer was concentrated in vacuum

출처 및 근거

ORD 기록
ord-3115b032009d46d58441cf76189fdca9
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09164384B2

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