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

HRID 1431380ノート

反応式

HRID 1431380 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 596310462,5-Dimorpholinopyridin-3-amine

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-516f140b145f4443ae1f13c87e1c22fa
出典データセット
uspto-grants-2015_01
特許番号
US08940724B2

反応ノート

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