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Potassium Nitrate → HCID 178430971、化合物

HRID 968797
ノート
印刷プレビュー

反応式

HRID 968797 の反応式
[CH3:1][C:2]1[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[C:5]([C:11]([OH:13])=[O:12])=[CH:4][CH:3]=1.[N+:14]([O-])([O-:16])=[O:15].[K+]>OS(O)(=O)=O>[CH3:1][C:2]1[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[C:5]([C:11]([OH:13])=[O:12])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15]
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

4

反応物 2

HCID 24434Potassium NitrateHCID 178425875HCID 178425875、化合物

生成物 1

HCID 178430971HCID 178430971、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
60 °C

実験手順

A mixture of 7-Methyl-1H-benzimidazole-4-carboxylic Acid (22) (4.944 g, 28.10 mmol) and concentrated H2SO4 (30 mL) is heated to about 60° C. to obtain a solution which is then cooled to about 0° C. To this solution is added KNO3 (3.12 g, 30.9 mmol) portionwise, so as to maintain the internal reaction temperature <10° C. Following complete addition, the cooling source is removed and the reaction mixture is allowed to warm to ambient temperature, whereupon the mixture is stirred for about 1 hour. The reaction mixture is then added to ice water (100 mL) and held at about 0° C. for about 4 hours. The resulting solids are filtered, washed with water, and dried to provide 7-Methyl-6-nitro-1H-benzimidazole-4-carboxylic Acid (23) as an off white solid (6.12 g, 98% Yield).

後処理

  1. customto obtain a solution which
  2. temperatureis then cooled to about 0° C
  3. temperatureso as to maintain the internal reaction temperature <10° C
  4. additionaddition
  5. customthe cooling source is removed
  6. temperatureto warm to ambient temperature, whereupon the mixture
  7. additionThe reaction mixture is then added to ice water (100 mL)
  8. waitheld at about 0° C. for about 4 hours
  9. filtrationThe resulting solids are filtered
  10. washwashed with water
  11. customdried

出典と根拠

ORDレコード
ord-8a579263fe334b0b862c26c8cebb94e8
出典データセット
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07304084B2

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