Morpholine → 8-Morpholino-1,7-naphthyridin-6-amine

HRID 2308599ノート

反応式

HRID 2308599 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10](Br)[N:11]=1)[N:8]=[CH:7][CH:6]=[CH:5]2.[NH:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1>CO>[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([N:13]3[CH2:18][CH2:17][O:16][CH2:15][CH2:14]3)[N:11]=1)[N:8]=[CH:7][CH:6]=[CH:5]2

参加物

4

反応物 2

HCID 8083MorpholineHCID 107043358-Bromo-1,7-naphthyridin-6-amine

生成物 1

HCID 139243758-Morpholino-1,7-naphthyridin-6-amine収率 60.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a mixture of 800 mg of 6-amino-8-bromo-1,7-naphthyridine and 3.12 g of morpholine, 40 ml of methanol was added. The resultant mixture was refluxed for 13 hours. After the reaction, methanol was distilled off under reduced pressure and chloroform was added to the residue. After washing the chloroform solution with water, it was dried with anhydrous magnesium sulfate. Chloroform was distilled off under reduced pressure and a small amount of acetone was added to the residue to dissolve same. Hexane was then added to the residue, followed by removal of insoluble matter by filtration. The filtrate was concentrated and the residue was recrystallized from a mixed solvent of chloroform and hexane, thereby obtaining 500 mg of 6-amino-8-morpholino-1,7-naphthyridine (Compound No. 3) as yellowish crystals (yield: 60.9%).

後処理

  1. additionwas added
  2. distillationwas distilled off under reduced pressure and chloroform
  3. additionwas added to the residue
  4. washAfter washing the chloroform solution with water, it
  5. dry with materialwas dried with anhydrous magnesium sulfate
  6. distillationChloroform was distilled off under reduced pressure
  7. additiona small amount of acetone was added to the residue
  8. dissolutionto dissolve same
  9. additionHexane was then added to the residue
  10. customfollowed by removal of insoluble matter by filtration
  11. concentrationThe filtrate was concentrated
  12. customthe residue was recrystallized from a mixed solvent of chloroform and hexane

出典と根拠

ORDレコード
ord-eea51c97601e4807b78320405ddd79ff
出典データセット
uspto-grants-1987_09
特許番号
US04690924

反応ノート

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