Nitric Acid → 6-Amino-5-nitropyridine-3-sulfonic acid

HRID 1520716ノート

反応式

HRID 1520716 の反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([S:8]([OH:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[N+:12]([O-])([OH:14])=[O:13]>OS(O)(=O)=O>[NH2:1][C:2]1[N:7]=[CH:6][C:5]([S:8]([OH:11])(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 4595336-Aminopyridine-3-sulfonic acid

生成物 1

HCID 203244826-Amino-5-nitropyridine-3-sulfonic acid

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
50 °C

実験手順

6-Aminopyridine-3-sulfonic acid (20 g) in concentrated H2SO4 (80 mL) was heated at 50° C. until it was completely dissolved. To this solution was added fuming HNO3 dropwise over 20 minutes. The rate of addition was kept slow so that the internal temperature did not exceeded 55° C. After the addition was complete, the reaction mixture was heated at 50° C. for 1 hour. After the mixture cooled to room temperature, it was poured into 150 g of ice. The mixture was stirred for another 1 hour. The whole flask was cooled to 0° C., and was kept at 0° C. for another 2 hours. The solid was collected by filtration, and was washed with cold 1:1 water/ethanol (20 mL), followed by diethyl ether (10 mL). The solid was dried in a vacuum oven overnight to give the title compound.

後処理

  1. dissolutionwas completely dissolved
  2. additionTo this solution was added
  3. customdropwise over 20 minutes
  4. additionThe rate of addition
  5. customdid not exceeded 55° C
  6. additionAfter the addition
  7. temperatureAfter the mixture cooled to room temperature
  8. temperatureThe whole flask was cooled to 0° C.
  9. waitwas kept at 0° C. for another 2 hours
  10. filtrationThe solid was collected by filtration
  11. washwas washed with cold 1:1 water/ethanol (20 mL)
  12. customThe solid was dried in a vacuum oven overnight

出典と根拠

ORDレコード
ord-edea7b13324e4044bd61a7dfc50c81d7
出典データセット
uspto-grants-2015_07
特許番号
US09073855B2

反応ノート

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