Ammonium formate → 3-Fluoro-4-morpholinoaniline

HRID 245306

반응식

HRID 245306 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 14853303-Fluoro-4-morpholinoaniline수율 95%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1c93aff449f8492a9eec693a741f577d
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658789B2

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