Allyl Alcohol → 4-{3-[(Prop-2-en-1-yl)oxy]pyrazin-2-yl}morpholine

HRID 1701735

반응식

HRID 1701735 반응식
Cl[C:2]1[C:7]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[N:6][CH:5]=[CH:4][N:3]=1.[CH2:14]([OH:17])[CH:15]=[CH2:16].[H-].[Na+]>CN(C)P(=O)(N(C)C)N(C)C>[CH2:14]([O:17][C:2]1[C:7]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[N:6][CH:5]=[CH:4][N:3]=1)[CH:15]=[CH2:16]

참가 물질

5

반응물 3

HCID 7858Allyl AlcoholHCID 24758Sodium hydride2회HCID 205289944-(3-Chloropyrazin-2-YL)morpholine

생성물 1

HCID 570676354-{3-[(Prop-2-en-1-yl)oxy]pyrazin-2-yl}morpholine

시약·촉매·용매 1

HCID 12679Hexamethylphosphoramide용매

반응 조건

온도
0 °C

실험 절차

120 g of 2-chloro-3-morpholinyl-pyrazine and 70 g of allyl alcohol are dissolved in 640 ml of hexamethylphosphoric acid triamide. 28.8 g of sodium hydride are introduced into this solution over the course of 30 minutes at 0° C. The mixture is then stirred for a further hour at 0° C. and thereafter for 1 hour at 30° C. and 15 hours at room temperature, until the reaction has subsided. The reaction mixture is then poured out onto 2 liters of ice water. After the excess sodium hydride present has been decomposed, the mixture is extracted by shaking with ether. The ether extracts are washed with water until neutral, dried over sodium sulphate and evaporated in a waterpump vacuum. The residue is distilled in a high vacuum. 2-Allyloxy-3-morpholinyl-pyrazine, boiling point 105°-106° C./0.03 mm Hg, is thus obtained.

후처리

  1. custom15 hours
  2. customat room temperature
  3. extractionthe mixture is extracted
  4. stirringby shaking with ether
  5. washThe ether extracts are washed with water until neutral,
  6. dry with materialdried over sodium sulphate
  7. customevaporated in a waterpump vacuum
  8. distillationThe residue is distilled in a high vacuum

출처 및 근거

ORD 기록
ord-4a7d77d451de4beb854b52acf32445a8
출처 데이터셋
uspto-grants-1980_03
특허 번호
US04195090

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