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Water → HCID 86591618, 화합물

HRID 1295701
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HRID 1295701 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[F:6][C:7]1[CH:12]=[C:11]([F:13])[C:10]([F:14])=[CH:9][C:8]=1[CH2:15][CH2:16][CH2:17][OH:18].C(N(CC)CC)C.O>ClCCl>[CH3:1][S:2]([O:18][CH2:17][CH2:16][CH2:15][C:8]1[CH:9]=[C:10]([F:14])[C:11]([F:13])=[CH:12][C:7]=1[F:6])(=[O:4])=[O:3]
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참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 199916093-(2,4,5-Trifluorophenyl)propan-1-ol

생성물 1

HCID 86591618HCID 86591618, 화합물수율 102.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Methanesulfonyl chloride (0.45 g, 3.88 mmol) was added dropwise to a solution of 3-(2,4,5-trifluorophenyl)propan-1-ol (0.46 g, 2.41 mmol; from Step 2) and triethylamine (0.71 g, 7.0 mmol) in dichloromethane (5 mL) at 0° C. The mixture was stirred at room temperature for 2 h. After complete disappearance of the alcohol (HPLC monitoring), dichloromethane (10 mL) and water (10 mL) were added. The aqueous phase was saturated with NaCl and extraction performed. The organic layer was washed with brine, dried over Na2SO4 and concentrated in vacuo to give 0.66 g (100%) of the title compound as a yellow oil. Purity by HPLC: 87%. This material was used directly in the next step.

후처리

  1. extractionThe aqueous phase was saturated with NaCl and extraction
  2. washThe organic layer was washed with brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-15a1c5a34cd34330855992608f0d51ce
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07244722B2

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