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Water → 1-Methanesulfonyloxy-4,4,5,5,6,6,7,7,7-nonafluoroheptane

HRID 1267467
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HRID 1267467 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[F:6][C:7]([F:22])([C:12]([F:21])([F:20])[C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15])[CH2:8][CH2:9][CH2:10][OH:11].C(N(CC)CC)C.O>ClCCl>[CH3:1][S:2]([O:11][CH2:10][CH2:9][CH2:8][C:7]([F:22])([F:6])[C:12]([F:20])([F:21])[C:13]([F:18])([F:19])[C:14]([F:15])([F:16])[F:17])(=[O:4])=[O:3]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 27790914,4,5,5,6,6,7,7,7-Nonafluoro-1-heptanol

생성물 1

HCID 120167731-Methanesulfonyloxy-4,4,5,5,6,6,7,7,7-nonafluoroheptane수율 92.2%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

실험 절차

Methanesulfonyl chloride (2.8 ml, 36.72 mmol) was added to a solution of 4,4,5,5,6,6,7,7,7-nonafluoroheptan-1-ol (6.0 g, 21.6 mmol) and triethylamine (6.0 ml, 43.2 mmol) in dichloromethane (60 ml) at 0° C., followed by stirring for 1 hour. After the reaction was completed, water was added to the reaction mixture, which was then extracted with dichloromethane. The organic layer was washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. After distilling off the solvent, the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/3) to give 1-methanesulfonyloxy-4,4,5,5,6,6,7,7,7-nonafluoroheptane (6.73 g, Yield 92.2%) as a colorless oil.

후처리

  1. extractionwas then extracted with dichloromethane
  2. washThe organic layer was washed with water and saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationAfter distilling off the solvent
  5. customthe residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/3)

출처 및 근거

ORD 기록
ord-972a09ee2dd64302abb7e85042eaaa7b
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06552069B1

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