Stannous chloride dihydrate → 2,5-Dimorpholinopyridin-3-amine

HRID 1431380노트

반응식

HRID 1431380 반응식
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:8]=[C:9]([N+:19]([O-])=O)[C:10]([N:13]3[CH2:18][CH2:17][O:16][CH2:15][CH2:14]3)=[N:11][CH:12]=2)[CH2:3][CH2:2]1.O.O.[Sn](Cl)Cl>CCOC(C)=O>[O:16]1[CH2:17][CH2:18][N:13]([C:10]2[C:9]([NH2:19])=[CH:8][C:7]([N:4]3[CH2:3][CH2:2][O:1][CH2:6][CH2:5]3)=[CH:12][N:11]=2)[CH2:14][CH2:15]1

참가 물질

4

반응물 2

HCID 61436Stannous chloride dihydrateHCID 596312774-(5-Morpholino-3-nitropyridin-2-yl)morpholine

생성물 1

HCID 596310462,5-Dimorpholinopyridin-3-amine

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a stirring solution of 4-(5-morpholino-3-nitropyridin-2-yl)morpholine (1.22 g, 4.15 mmol; described herein) and EtOAc (50 mL) was added tin(II) chloride dihydrate (4.52 g, 20.7 mmol). The mixture was stirred at rt for ten min, refluxed for 2 h, and then cooled to rt. A solid was removed by filtration and both this and the EtOAc solution were washed with water and brine. The combined aq. portions were basified with 1M NaOH and the product extracted with EtOAc, dried (magnesium sulfate), and concentrated, affording 2,5-dimorpholinopyridin-3-amine as a beige solid. Mass Spectrum (ESI) m/e=265.2 (M+1).

후처리

  1. temperaturerefluxed for 2 h
  2. temperaturecooled to rt
  3. customA solid was removed by filtration
  4. washboth this and the EtOAc solution were washed with water and brine
  5. extractionthe product extracted with EtOAc
  6. dry with materialdried (magnesium sulfate)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-516f140b145f4443ae1f13c87e1c22fa
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08940724B2

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