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

HRID 1764327
ノート
印刷プレビュー

反応式

HRID 1764327 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7858Allyl AlcoholHCID 24758Sodium hydride2 回HCID 204834273-Chloro-N,N-dimethylpyrazin-2-amine

生成物 1

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

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-42943661e90d446f857b2d56334a17b6
出典データセット
uspto-grants-1978_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04115575

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート