Water → 3-Fluoropropyl methanesulfonate

HRID 1087356노트

반응식

HRID 1087356 반응식
[F:1][CH2:2][CH2:3][CH2:4][OH:5].C(N(CC)CC)C.[CH3:13][S:14](Cl)(=[O:16])=[O:15].O>C(Cl)Cl>[CH3:13][S:14]([O:5][CH2:4][CH2:3][CH2:2][F:1])(=[O:16])=[O:15]

참가 물질

6

실험 절차

To an ice cold, stirred solution of 19.0 g (0.244 mole) of 3-fluoropropanol and 39.5 g (0.300 mole) of triethylamine in 300 mL of methylene chloride was added dropwise 34.4 g (0.300 mole) of methanesulfonyl chloride. The resultant mixture was allowed to warm to room temperature and was stirred for approximately 18 hours. The mixture was poured into water and was washed with an aqueous, saturated sodium bicarbonate solution. The organic phase was dried over anhydrous magnesium sulfate and was filtered. The filtrate was distilled under reduced pressure to yield 41.3 g of 3-fluoropropyl methanesulfonate as a liquid, bp 116° C./15 mm Hg.

후처리

  1. washwas washed with an aqueous, saturated sodium bicarbonate solution
  2. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  3. filtrationwas filtered
  4. distillationThe filtrate was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-d0d60b880939475fb91ef69a1ac6be78
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05035740

반응 노트

불러오는 중…