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

HRID 459945ノート

反応式

HRID 459945 の反応式
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]

参加物

3

反応物 1

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

生成物 1

HCID 102618922,6-Difluoro-3,5-dimethoxybenzenamine収率 97%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f425581ce63947c2a19ca9b8f355ec1f
出典データセット
uspto-grants-2007_03
特許番号
US07196090B2

反応ノート

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