Ammonium formate → 3-Fluoro-4-morpholinoaniline

HRID 245306

反応式

HRID 245306 の反応式
[F:1][C:2]1[CH:3]=[C:4]([N+:14]([O-])=O)[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1.C([O-])=O.[NH4+]>C(OCC)(=O)C.[Pd]>[F:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1)[NH2:14]

参加物

5

反応物 2

HCID 2723923Ammonium formateHCID 29054894-(2-Fluoro-4-nitrophenyl)morpholine

生成物 1

HCID 14853303-Fluoro-4-morpholinoaniline収率 95%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

10% Pd—C 4.0 g was added to 3-fluoro-4-morpholinyl nitrobenzene (40 g, 177 mmol), ammonium formate (50 g, 793 mmol) in 200 mL of ethyl acetate and stirred at 45˜50° C. for 8 h until the completion of the reaction. The mixture was then filtrated and separated by water. The organic layer was washed with brine and dried over anhydrous magnesium sulfate, filtered, and the solvent was evaporated to provide 33 g of solid in 95% yield.

後処理

  1. filtrationThe mixture was then filtrated
  2. customseparated by water
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-1c93aff449f8492a9eec693a741f577d
出典データセット
uspto-grants-2014_02
特許番号
US08658789B2

関連ノート

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