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Chloroform → HCID 22662826、化合物

HRID 392305
ノート
印刷プレビュー

反応式

HRID 392305 の反応式
N[C:2]1[N:7]=[C:6]([C:8]([NH2:10])=[O:9])[C:5]([O:11][CH3:12])=[N:4][CH:3]=1.N([O-])=O.[Na+].C(Cl)(Cl)Cl.N1C=CC=CC=1.[FH:27]>>[F:27][C:2]1[N:7]=[C:6]([C:8]([NH2:10])=[O:9])[C:5]([O:11][CH3:12])=[N:4][CH:3]=1
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 4

HCID 6212ChloroformHCID 64774Pyridine, hydrofluoride (1:1)HCID 226628026-Amino-3-methoxy-2-pyrazinecarboxamideHCID 23668193Sodium Nitrite

生成物 1

HCID 22662826HCID 22662826、化合物

反応条件

温度
10 °C

実験手順

In an atmosphere of nitrogen gas, 1.50 g of 6-amino-3-methoxy-2-pyrazinecarboxamide was dissolved in 12 mL of 70% hydrogen fluoride-pyridine solution at an ice-cooled temperature. Then, 0.71 g of sodium nitrite was added at −50° C., and the mixture thus obtained was stirred at 10° C. for one hour. After stirring the reaction mixture for an additional one hour, a mixture of 50 mL of ice water and 100 mL of chloroform was added, and the mixture thus obtained was separated into layers. The organic layer was washed with saturated aqueous solution of sodium chloride and dried on anhydrous magnesium sulfate and the solvent was removed under reduced pressure. Thus, 1.29 g of 6-fluoro-3-methoxy-2-pyrazinecarboxamide was obtained as a solid product.

後処理

  1. temperaturecooled temperature
  2. customthe mixture thus obtained
  3. stirringAfter stirring the reaction mixture for an additional one hour
  4. additionwas added
  5. customthe mixture thus obtained
  6. customwas separated into layers
  7. washThe organic layer was washed with saturated aqueous solution of sodium chloride
  8. dry with materialdried on anhydrous magnesium sulfate
  9. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-0cc52b76adc5400d90a24db69d6b3bd2
出典データセット
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06800629B2

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