Trifluoroacetic acid → 2-Fluoro-3,5-dimethoxyaniline

HRID 459948ノート

反応式

HRID 459948 の反応式
C(OC(=O)[NH:7][C:8]1[CH:13]=[C:12]([O:14][CH3:15])[CH:11]=[C:10]([O:16][CH3:17])[C:9]=1[F:18])(C)(C)C.FC(F)(F)C(O)=O>>[F:18][C:9]1[C:10]([O:16][CH3:17])=[CH:11][C:12]([O:14][CH3:15])=[CH:13][C:8]=1[NH2:7]

参加物

3

反応物 2

HCID 6422Trifluoroacetic acidHCID 69030856tert-Butyl (2-fluoro-3,5-dimethoxyphenyl)carbamate

生成物 1

HCID 153245152-Fluoro-3,5-dimethoxyaniline収率 95.5%

実験手順

To 56.6 g (0.21 mol) of (2-fluoro-3,5-dimethoxy-phenyl)-carbamic acid tert-butyl ester, 184 mL of trifluoroacetic acid was added to give a homogeneous solution which was stirred at room temperature for 30 minutes. After 30 minutes, 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 two times with diethylether. The combined diethylether layers were washed one time with brine, dried over sodium sulfate, filtered and evaporated to give 34.1 g (95.5%) of title compound. MS (APCI) (m+1)/z 172.0.

後処理

  1. customto give a homogeneous solution which
  2. waitAfter 30 minutes
  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 two times with diethylether
  6. washThe combined diethylether layers were washed one time with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated

出典と根拠

ORDレコード
ord-d016498d2be840c49c8f8d867d4f0593
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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