Sodium hydride → HCID 131711265、化合物

HRID 647966ノート

反応式

HRID 647966 の反応式
Cl[C:2]1[C:7]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[N:6][C:5]([CH3:14])=[CH:4][N:3]=1.C1(C2[N:25]([CH:26]([CH3:28])[CH3:27])[CH2:24][CH:23]([CH2:29][OH:30])[O:22]2)C=CC=CC=1.[H-].[Na+]>CN(C)P(=O)(N(C)C)N(C)C>[CH:26]([NH:25][CH2:24][CH:23]([OH:22])[CH2:29][O:30][C:2]1[C:7]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[N:6][C:5]([CH3:14])=[CH:4][N:3]=1)([CH3:28])[CH3:27]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 125661982-Phenyl-3-isopropyl-5-hydroxymethyloxazolidineHCID 570620344-(3-Chloro-6-methylpyrazin-2-yl)morpholine

生成物 1

HCID 131711265HCID 131711265、化合物

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒

実験手順

10.7 g of 2-chloro-3-morpholinyl-5-methyl-pyrazine and 16.6 g of 2-phenyl-3-isopropyl-5-hydroxymethyloxazolidine are dissolved in 130 ml of hexamethylphosphoric acid triamide. 3.6 g of a 50% strength suspension of sodium hydride in paraffin oil are introduced into this solution over the course of 30 minutes at 0°-5° C., whilst stirring. The mixture is then stirred for 1 hour at 0°-5° C. and 24 hours at room temperature. The reaction mixture is then poured onto 500 ml of ice water and extracted by shaking with ether. The ether extracts are washed with water and evaporated in a waterpump vacuum. The residue is taken up in 200 ml of 1 N sulphuric acid and the reaction mixture is stirred for 15 hours at room temperature and then extracted by shaking with ether. The acid aqueous phase is rendered alkaline with concentrated sodium hydroxide solution and is then extracted by shaking with ether. The ether extracts are washed with water, dried over sodium sulphate and evaporated in a waterpump vacuum. The residue crystallises from ether-pentane. 2-(3'-Isopropylamino-2'-hydroxy-propoxy)-3-morpholinyl-5-methyl-pyrazine, melting point 77°-78° C., is thus obtained.

後処理

  1. additionare introduced into this solution over the course of 30 minutes at 0°-5° C.
  2. stirringThe mixture is then stirred for 1 hour at 0°-5° C. and 24 hours at room temperature
  3. extractionextracted
  4. stirringby shaking with ether
  5. washThe ether extracts are washed with water
  6. customevaporated in a waterpump vacuum
  7. stirringthe reaction mixture is stirred for 15 hours at room temperature
  8. extractionextracted
  9. stirringby shaking with ether
  10. extractionis then extracted
  11. stirringby shaking with ether
  12. washThe ether extracts are washed with water
  13. dry with materialdried over sodium sulphate
  14. customevaporated in a waterpump vacuum
  15. customThe residue crystallises from ether-pentane

出典と根拠

ORDレコード
ord-e46afa4786824886995de4b7ec330690
出典データセット
uspto-grants-1983_10
特許番号
US04410530

反応ノート

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