Dibromodifluoromethane → 4-Bromo-4,4-difluorobutanoic acid

HRID 2399725노트

반응식

HRID 2399725 반응식
[C:1]([OH:5])(=[O:4])[CH:2]=[CH2:3].S(S([O-])=O)([O-])=O.[Na+].[Na+].C(=O)(O)[O-].[Na+].[Br:19][C:20](Br)([F:22])[F:21]>C(OCC)(=O)C.O.C(#N)C>[Br:19][C:20]([F:22])([F:21])[CH2:3][CH2:2][C:1]([OH:5])=[O:4]

참가 물질

8

실험 절차

To a stirred solution of acrylic acid (1.44 g) and acetonitrile (80 cm3) was added sodium dithionite (4.18 g), sodium bicarbonate (2.01 g), water (20 cm3) and finally dibromodifluoromethane (5 cm3). The biphasic mixture was stirred at the ambient temperature with the inorganic salts gradually dissolving. Gc analysis after 4 hrs indicated complete consumption of acrylic acid. The aqueous phase was saturated with solid sodium chloride. The organic phase was separated, dried (MgSO4), filtered and evaporated under reduced pressure to give a pale yellow oil with a small amount of a white solid. This mixture was taken up in ethyl acetate, filtered and evaporated under reduced pressure to give a pale yellow oil (2.54 g). 1H NMR (DMSO): δ2.65(2H,m); 2.45(2H, t).

후처리

  1. dissolutiongradually dissolving
  2. customconsumption of acrylic acid
  3. customThe organic phase was separated
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customto give a pale yellow oil with a small amount of a white solid
  8. filtrationfiltered
  9. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-26284fce89974f5584123fe512529bbb
출처 데이터셋
uspto-grants-1995_09
특허 번호
US05451594

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