Water → 2,4,5-Trifluorophenylacetic acid

HRID 76846

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HRID 76846 반응식
S(=O)(=O)(O)O.Cl[C:7]#[C:8][C:9]1[CH:14]=[C:13]([F:15])[C:12]([F:16])=[CH:11][C:10]=1[F:17].CC([O:22]C)(C)C.[OH2:24]>>[F:17][C:10]1[CH:11]=[C:12]([F:16])[C:13]([F:15])=[CH:14][C:9]=1[CH2:8][C:7]([OH:22])=[O:24]

참가 물질

5

반응물 4

HCID 962WaterHCID 1118Sulfuric AcidHCID 15413tert-Butyl methyl etherHCID 86343656HCID 86343656, 화합물

생성물 1

HCID 27779502,4,5-Trifluorophenylacetic acid수율 25%

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온도
100 °C

실험 절차

50 ml of concentrated sulphuric acid was added to 1-chloroethynyl-2,4,5-trifluorobenzene of formula IV, X═Cl and the mixture heated to 100° C. and left to stir for 1 hour. 50 ml of MTBE and 100 ml of water were then added. The phases were separated and the aqueous phase was re-extracted with 2×50 ml of MTBE. The combined organic phases were counter extracted with 3×50 ml of aqueous NaHCO3 and put to one side. The three aqueous phases of NaHCO3 were recombined and the resulting phase was acidified with hydrochloric acid and then extracted with 3×50 ml of MTBE. The organic phases were concentrated to a residue obtaining 0.25 g of 2,4,5-trifluorophenylacetic acid of formula (I) with a molar yield of 25%.

후처리

  1. waitleft
  2. customThe phases were separated
  3. extractionthe aqueous phase was re-extracted with 2×50 ml of MTBE
  4. extractionThe combined organic phases were counter extracted with 3×50 ml of aqueous NaHCO3
  5. extractionextracted with 3×50 ml of MTBE
  6. concentrationThe organic phases were concentrated to a residue

출처 및 근거

ORD 기록
ord-266f8b4c0c3344e69418dd7c1bdcc3b4
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835679B2

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