Hydrochloric Acid → HCID 178506234, 화합물

HRID 1009161

반응식

HRID 1009161 반응식
CCO.Cl.[CH2:5]([NH:12]/[C:13](/[C:21]1[CH:26]=[C:25]([Br:27])[CH:24]=[CH:23][C:22]=1[OH:28])=[CH:14]\[C:15](=O)[C:16]([F:19])([F:18])[F:17])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>O.N.CCOC(C)=O>[Br:27][C:25]1[CH:26]=[C:21]2[C:22](=[CH:23][CH:24]=1)[O:28][C:15]([C:16]([F:18])([F:19])[F:17])=[CH:14]/[C:13]/2=[N:12]/[CH2:5][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 67304920(Z)-4-(benzylamino)-4-(5-bromo-2-hydroxyphenyl)-1,1,1-trifluorobut-3-en-2-one

생성물 1

HCID 178506234HCID 178506234, 화합물

시약·촉매·용매 3

HCID 222Ammonia용매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To a cooled (ice bath) EtOH (96 ml) was bubbled through hydrogen chloride gas for 30 min. (Z)-4-(benzylamino)-4-(5-bromo-2-hydroxyphenyl)-1,1,1-trifluorobut-3-en-2-one (24.0 g, 60 mmol) was then added in one portion to this solution. The reaction was stirred at RT for 36 h. The resulted mixture was diluted with 900 ml of cool water, 28% aq NH3 (96 ml) was then added. The precipitate formed was filtered and washed with water to give a brown sticky solid. The solid was dissolved in EtOAc, washed with 1N HCl and brine. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was crystallized from hexane to give the title compound as a brown solid. MS m/z: 382.

후처리

  1. additionwas then added in one portion to this solution
  2. additionwas then added
  3. customThe precipitate formed
  4. filtrationwas filtered
  5. washwashed with water
  6. customto give a brown sticky solid
  7. washwashed with 1N HCl and brine
  8. dry with materialThe organic layer was dried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe residue was crystallized from hexane

출처 및 근거

ORD 기록
ord-14124da969ab465ab56f57c7f3686a9b
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07973047B2

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