Water → 1-Fluoromethyl-2-phenylethyl methanesulfonate

HRID 749297노트

반응식

HRID 749297 반응식
[F:1][CH2:2][CH:3]([OH:11])[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.C(N(CC)CC)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21].O>C(Cl)Cl>[CH3:19][S:20]([O:11][CH:3]([CH2:2][F:1])[CH2:4][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1)(=[O:22])=[O:21]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 2300811-Fluoro-3-phenylpropan-2-ol

생성물 1

HCID 866014541-Fluoromethyl-2-phenylethyl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of 1-fluoromethyl-2-phenylethanol (1.0 g, prepared as described by Bergmann, et al., J. Chem. Soc., 1961, 3448-3452) in DCM (30 mL) at 0° C. under nitrogen was added triethylamine (1.36 mL) followed by dropwise addition of methanesulfonyl chloride (0.6 mL). The mixture was allowed to slowly warm to room temperature overnight. The reaction mixture was poured into water and extracted with EtOAc. The EtOAc extracts were washed with water and brine, dried over Na2SO4, and concentrated to dryness to give 1.3 g of the title compound. MS CI, (M++H)=233, (M++H −CH3SO3H)=138.

후처리

  1. extractionextracted with EtOAc
  2. washThe EtOAc extracts were washed with water and brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-b56c99b5d05849bd8c26bac955d37463
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07402604B2

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