2-Aminopyridine → 6-Aminopyridine-3-sulfonic acid

HRID 1068680ノート

反応式

HRID 1068680 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[OH:8][S:9](O)(=[O:11])=[O:10].O=S(=O)=O>>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:9]([OH:11])(=[O:10])=[O:8])=[CH:4][N:3]=1

参加物

3

反応物 2

HCID 104392-AminopyridineHCID 24681Fuming sulfuric acid

生成物 1

HCID 4595336-Aminopyridine-3-sulfonic acid収率 75.2%

反応条件

温度
140 °C

実験手順

2-Aminopyridine (80 g, 0.85 mol) was added portionwise over 30 minutes to stirred oleum (320 g) and the resulting solution heated at 140° C. for 4 hours, then allowed to cool. The reaction mixture was poured onto stirred ice (200 g) and this mixture stirred at ice-salt bath temperature for a further 2 hours. The resulting suspension was filtered, then the collected solid washed successively with ice-water (200 ml) and cold industrial methylated spirit (IMS) (200 ml) and, finally, dried under suction to provide the title compound (111.3 g, 75%) as a solid. LRMS: m/z 175 (M+1)+.

後処理

  1. temperatureto cool
  2. additionThe reaction mixture was poured
  3. filtrationThe resulting suspension was filtered
  4. washthe collected solid washed successively with ice-water (200 ml) and cold industrial methylated spirit (IMS) (200 ml)
  5. customfinally, dried under suction

出典と根拠

ORDレコード
ord-cbfe28f246674da2bbef7d36c4c702e0
出典データセット
uspto-grants-2001_06
特許番号
US06251904B1

反応ノート

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