Hydrochloric Acid → HCID 19705275, 화합물

HRID 727172

반응식

HRID 727172 반응식
[Mg].[F:2][C:3]1([F:16])[C:7]([F:9])([F:8])[C:6]2[CH:10]=[CH:11][CH:12]=[C:13]([Mg]Cl)[C:5]=2[O:4]1.C[CH:18](OC(C)=O)[O:19]C(C)=O.Cl.CCCCCCCC>C1(C)C=CC=CC=1>[F:2][C:3]1([F:16])[C:7]([F:9])([F:8])[C:6]2[CH:10]=[CH:11][CH:12]=[C:13]([CH2:18][OH:19])[C:5]=2[O:4]1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 356OctaneHCID 2225361,1-Ethanediol, 1,1-diacetateHCID 5462224MagnesiumHCID 178506009HCID 178506009, 화합물

생성물 1

HCID 19705275HCID 19705275, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Under a nitrogen atmosphere, the reaction mixture from above is decanted into a clean, dry reaction vessel, leaving the unreacted magnesium turnings in the first vessel. This solution containing 2,2,3,3-tetrafluoro-2,3-dihydrobenzofuran-7-ylmagnesium chloride is heated at reflux, and 16.5 grams (0.55 mole based on formaldehyde) of polyoxymethylene diacetate (avg. mol. wgt. approx. 50,000, commercially available from E. I. du Pont De Nemours & Co., Inc. Wilmington Del., under the trade name Delrin 500 acetal homopolymer resin), milled to about 80 mesh, is added with stirring during about a three hour period. Upon completion of addition, the reaction mixture is heated at reflux for an additional four hours and then is allowed to cool to ambient temperature as it stood for about 18 hours. The reaction mixture is warmed to about 53° C. and then is poured into 100 grams of ice, 52 grams of concentrated hydrochloric acid, and 200 grams of a mixture of 95% n-octane and 5% toluene (wt/wt). This mixture is filtered, and the organic layer is separated. The organic layer is concentrated under reduced pressure, yielding 2,2,3,3-tetrafluoro-2,3-dihydrobenzofuran-7-ylmethanol.

후처리

  1. customUnder a nitrogen atmosphere, the reaction mixture from above is decanted into a clean,
  2. customdry
  3. customreaction vessel
  4. temperatureis heated
  5. temperatureat reflux
  6. additionis added
  7. additionUpon completion of addition
  8. temperaturethe reaction mixture is heated
  9. temperatureat reflux for an additional four hours
  10. waitstood for about 18 hours
  11. temperatureThe reaction mixture is warmed to about 53° C.
  12. filtrationThis mixture is filtered
  13. customthe organic layer is separated
  14. concentrationThe organic layer is concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-eb8dc086490948328eef38c2e3e2bf3b
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05712281

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