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Triethylamine → 2-(2,4-Difluorophenyl)ethyl methanesulphonate

HRID 1891304
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HRID 1891304 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].C(N(CC)CC)C.[F:13][C:14]1[CH:19]=[C:18]([F:20])[CH:17]=[CH:16][C:15]=1[CH2:21][CH2:22][OH:23]>ClCCl>[CH3:1][S:2]([O:23][CH2:22][CH2:21][C:15]1[CH:16]=[CH:17][C:18]([F:20])=[CH:19][C:14]=1[F:13])(=[O:4])=[O:3]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 534034612-(2,4-Difluorophenyl)ethanol

생성물 1

HCID 866397272-(2,4-Difluorophenyl)ethyl methanesulphonate수율 63.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

Methanesulphonyl chloride (3.3 ml; 0.043 mol) and triethylamine (5.9 ml; 0.043 mol) were added to a solution of 2-(2,4-difluorophenyl)ethanol (6.4 g; 0.0426 mol) in dichloromethane (100 ml). The solution was cooled for 1 h at 0° C. and then brought to room temperature for 1 h. The reaction mixture was then treated by washing, successively, with 5N sulphuric acid (20 ml), water (50 ml), a 5% solution of NaHCO3 (50 ml) and water (50 ml). The organic phase was then dried over Na2SO4, filtered and concentrated at reduced pressure. The residue was taken up twice in CCl4, thus obtaining 6.42 g of 2-(2,4-difluorophenyl)ethyl methanesulphonate.

후처리

  1. additionThe reaction mixture was then treated
  2. washby washing
  3. dry with materialThe organic phase was then dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated at reduced pressure

출처 및 근거

ORD 기록
ord-1ae1936b97a049c3bb1a06efe87e748e
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507528B2

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