(2,6-Difluoro-3,5-dimethoxy-phenyl)-carbamic Acid Tert-Butyl Ester → 2,6-Difluoro-3,5-dimethoxybenzenamine

HRID 459945노트

반응식

HRID 459945 반응식
C(OC(=O)[NH:7][C:8]1[C:13]([F:14])=[C:12]([O:15][CH3:16])[CH:11]=[C:10]([O:17][CH3:18])[C:9]=1[F:19])(C)(C)C>FC(F)(F)C(O)=O>[F:14][C:13]1[C:12]([O:15][CH3:16])=[CH:11][C:10]([O:17][CH3:18])=[C:9]([F:19])[C:8]=1[NH2:7]

참가 물질

3

반응물 1

HCID 86590945(2,6-Difluoro-3,5-dimethoxy-phenyl)-carbamic Acid Tert-Butyl Ester

생성물 1

HCID 102618922,6-Difluoro-3,5-dimethoxybenzenamine수율 97%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

To 34.6 g (0.12 mol) of (2,6-difluoro-3,5-dimethoxy-phenyl)-carbamic acid tert-butyl ester, 120 mL of trifluoroacetic acid was added to give a homogeneous solution which was stirred at room temperature for 30 minutes. After 30 min., the reaction mixture was concentrated in vacuo. To the residue, a saturated solution of sodium bicarbonate was carefully added to pH 8. The resulting suspension was extracted twice with diethylether. Combined diethylether layers were washed once with brine, dried over sodium sulfate, filtered and evaporated to give 22 g (97%) of title compound. MS (APCI) (m+1)/z 190.1.

후처리

  1. customto give a homogeneous solution which
  2. waitAfter 30 min.
  3. concentrationthe reaction mixture was concentrated in vacuo
  4. additionTo the residue, a saturated solution of sodium bicarbonate was carefully added to pH 8
  5. extractionThe resulting suspension was extracted twice with diethylether
  6. washCombined diethylether layers were washed once with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated

출처 및 근거

ORD 기록
ord-f425581ce63947c2a19ca9b8f355ec1f
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07196090B2

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