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Sulfuric Acid → HCID 178513826、化合物

HRID 392327
ノート
印刷プレビュー

反応式

HRID 392327 の反応式
S(=O)(=O)(O)O.[OH:6][C:7]1[C:8]([C:13]([NH2:15])=[O:14])=[N:9][CH:10]=[CH:11][N:12]=1.[N+:16]([O-])([O-:18])=[O:17].[K+].[OH-].[Na+]>O>[OH:6][C:7]1[C:8]([C:13]([NH2:15])=[O:14])=[N:9][C:10]([N+:16]([O-:18])=[O:17])=[CH:11][N:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 24434Potassium NitrateHCID 178513804HCID 178513804、化合物

生成物 1

HCID 178513826HCID 178513826、化合物収率 65.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Into 1.2 L of 97% sulfuric acid was added and dissolved 208.0 g of 3-hydroxy-2-pyrazinecarboxamide, while keeping the solution at 10-25° C. by cooling it with ice. To the solution thus obtained was added 185.0 g of potassium nitrate at 30-35° C., and the mixture thus obtained was stirred at room temperature for 15 hours and then at 40° C. for 2 hours. After cooling the reaction mixture to 20° C., it was poured into 6 L of ice water and stirred at room temperature for one hour, and the deposited matter was collected by filtration and washed with two 500 mL portions of water. The solid product thus obtained was suspended in 1 L of water, pH was adjusted to 1.5 with 5 mol/L aqueous solution of sodium hydroxide, and then the solid matter was collected by filtration. The solid was washed successively with 500 mL of water and 500 mL of acetone to obtain 180.0 g of 3-hydroxy-6-nitro-2-pyrazinecarboxamide as a solid product.

後処理

  1. customat 10-25° C.
  2. temperatureby cooling it with ice
  3. customTo the solution thus obtained
  4. customthe mixture thus obtained
  5. waitat 40° C. for 2 hours
  6. temperatureAfter cooling the reaction mixture to 20° C.
  7. stirringstirred at room temperature for one hour
  8. filtrationthe deposited matter was collected by filtration
  9. washwashed with two 500 mL portions of water
  10. customThe solid product thus obtained
  11. filtrationthe solid matter was collected by filtration
  12. washThe solid was washed successively with 500 mL of water and 500 mL of acetone

出典と根拠

ORDレコード
ord-1d87318ce02f435b8b746fab9ce21ee9
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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