Morpholino(3-nitrophenyl)methanone → 3-(Morpholine-4-carbonyl)aniline

HRID 2737

반응식

HRID 2737 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:15]=[CH:16][CH:17]=1)[C:7]([N:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1)=[O:8])([O-])=O>C(O)C.O.NN.[Pd]>[NH2:1][C:4]1[CH:5]=[C:6]([CH:15]=[CH:16][CH:17]=1)[C:7]([N:9]1[CH2:10][CH2:11][O:12][CH2:13][CH2:14]1)=[O:8]

참가 물질

5

반응물 1

HCID 225453Morpholino(3-nitrophenyl)methanone

생성물 1

HCID 64850643-(Morpholine-4-carbonyl)aniline수율 100.5%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매2회HCID 24654Hydrazine hydrate (1:1)용매

반응 조건

온도
50 °C

실험 절차

The compound ([13]-(132)-158) (8.63 g) prepared in Example 83 was dissolved in ethanol (400 ml), and the solution was heated to 50° C. To the suspention, a solution of 10% Pd/C (2.25 g) in ethanol and hydrazine monohydrate (4.4 ml) were added to the solution. The mixture was stirred for 30 minutes. After the reaction was completed, the catalyst was removed by filtration through celite. The solution was concentrated, and the residue was purified by silica gel column chromatography (Kieselgel 60=120 g, ethyl acetate) to obtain the above-captioned compound ([13]-(133)-158) (7.57 g) as a white solid.

후처리

  1. customthe catalyst was removed by filtration through celite
  2. concentrationThe solution was concentrated
  3. customthe residue was purified by silica gel column chromatography (Kieselgel 60=120 g, ethyl acetate)

출처 및 근거

ORD 기록
ord-7cc7d41500194b2d804cca39c54e96aa
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731310

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