Sodium hydride → HCID 131711265, 화합물

HRID 1764332노트

반응식

HRID 1764332 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 131711265HCID 131711265, 화합물

시약·촉매·용매 1

HCID 12679Hexamethylphosphoramide용매

실험 절차

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 etherpentane. 2-(3'-Isopropylamino-2'-hydroxy-propoxy)-3-morpholinyl-5-methyl-pyrazine, melting point 77°-78° C., is thus obtained.

후처리

  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 etherpentane

출처 및 근거

ORD 기록
ord-bc908eeff8b5419f8de84c61ac0b19b7
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04115575

반응 노트

불러오는 중…