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Allyl Alcohol → N,N-Dimethyl-3-[(prop-2-en-1-yl)oxy]pyrazin-2-amine

HRID 1764327
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HRID 1764327 반응식
Cl[C:2]1[C:7]([N:8]([CH3:10])[CH3:9])=[N:6][CH:5]=[CH:4][N:3]=1.[CH2:11]([OH:14])[CH:12]=[CH2:13].[H-].[Na+]>CN(C)P(=O)(N(C)C)N(C)C>[CH2:11]([O:14][C:2]1[C:7]([N:8]([CH3:10])[CH3:9])=[N:6][CH:5]=[CH:4][N:3]=1)[CH:12]=[CH2:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7858Allyl AlcoholHCID 24758Sodium hydride2회HCID 204834273-Chloro-N,N-dimethylpyrazin-2-amine

생성물 1

HCID 20483434N,N-Dimethyl-3-[(prop-2-en-1-yl)oxy]pyrazin-2-amine

시약·촉매·용매 1

HCID 12679Hexamethylphosphoramide용매

반응 조건

온도
0 °C

실험 절차

47 g of 2-chloro-3-dimethylamino-pyrazine and 35 g of allyl alcohol are dissolved in 300 ml of hexamethylphosphoric acid triamide. 14.4 g of sodium hydride are introduced into this solution at 0° C. over the course of 30 minutes. The mixture is then stirred for a further hour at 0° C. and for 15 hours at room temperature. The reaction mixture is then poured into 2 liters of ice water. After excess sodium hydride 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 under reduced pressure. 2-Allyloxy-3-dimethylamino-pyrazine, boiling point 110°-115° C./10 mm Hg, is thus obtained.

후처리

  1. extractionthe mixture is extracted
  2. stirringby shaking with ether
  3. washThe ether extracts are washed with water until neutral,
  4. dry with materialdried over sodium sulphate
  5. customevaporated in a waterpump vacuum
  6. distillationThe residue is distilled under reduced pressure

출처 및 근거

ORD 기록
ord-42943661e90d446f857b2d56334a17b6
출처 데이터셋
uspto-grants-1978_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04115575

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