Hydrochloric Acid → 4-Methyl-5-iodosaccharin

HRID 861822

反応式

HRID 861822 の反応式
Cl.[CH3:2][C:3]1[C:13](N)=[CH:12][CH:11]=[C:10]2[C:4]=1[C:5](=[O:15])[NH:6][S:7]2(=[O:9])=[O:8].N([O-])=O.[Na+].[I-:20].[K+]>O.C(O)(=O)C>[CH3:2][C:3]1[C:13]([I:20])=[CH:12][CH:11]=[C:10]2[C:4]=1[C:5](=[O:15])[NH:6][S:7]2(=[O:9])=[O:8]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 4875Potassium IodideHCID 23668193Sodium NitriteHCID 701876914-Methyl-5-aminosaccharin

生成物 1

HCID 153462934-Methyl-5-iodosaccharin

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回

実験手順

A mixture of 205 ml of glacial acetic acid, 160 ml of water and 40 ml of conc. HCl is initially taken and 23.4 g (0.11 mol) of 4-methyl-5-aminosaccharin are introduced with stirring at 15°-20° C. 7.9 g (0.115 mol) of sodium nitrite are added dropwise to the resulting suspension at 5°-10° C. and it is stirred at 5° C. for 30 min. The diazonium salt, which is present as a suspension, is then added dropwise in portions to a solution, which is warmed to 50° C., of 19.1 g (0.115 mol) of potassium iodide in 170 ml of water, nitrogen being formed. After cooling to room temperature, the deposited product is isolated by filtering off with suction, washed with water and dried under reduced pressure at 50° C. 32.5 g (0.1 mol=91% of theory) of a solid of m.p.: 257°-258° C. are obtained.

後処理

  1. stirringit is stirred at 5° C. for 30 min
  2. additionis then added dropwise in portions to a solution, which
  3. customformed
  4. customthe deposited product is isolated
  5. filtrationby filtering off with suction
  6. washwashed with water
  7. customdried under reduced pressure at 50° C
  8. custom32.5 g (0.1 mol=91% of theory) of a solid of m.p.: 257°-258° C. are obtained

出典と根拠

ORDレコード
ord-50933999bc3147b5a87b83045d98ad61
出典データセット
uspto-grants-1998_02
特許番号
US05716905

関連ノート

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