海萝胶 → 4-Methyl-5-iodosaccharin

HRID 343749

反应方程式

HRID 343749 反应方程式
Cl.[CH3:2][C:3]1[C:8]2[C:9](=[O:14])[NH:10][S:11](=[O:13])(=[O:12])[C:7]=2[CH:6]=[CH:5][C:4]=1N.N([O-])=O.[Na+].[I-:20].[K+]>O.C(O)(=O)C>[CH3:2][C:3]1[C:8]2[C:9](=[O:14])[NH:10][S:11](=[O:13])(=[O:12])[C:7]=2[CH:6]=[CH:5][C:4]=1[I:20]

参与物

7

反应物 4

HCID 313海萝胶HCID 4875碘化钾HCID 23668193亚硝酸钠HCID 701876914-Methyl-5-aminosaccharin

产物 1

HCID 153462934-Methyl-5-iodosaccharin

试剂、催化剂与溶剂 2

HCID 176醋酸溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂2 次

反应条件

温度
50 °C

实验过程

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-amino-1,1,3-trioxo-2,3-dihydro-1λ6 benz[d]isothiazole 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 of 19.1 g (0.115 mol) of potassium iodide in 170 ml of water which is warmed to 50° C., 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. A combustion analysis gave an iodine content of 38.5% (theory 39.3%).

后处理

  1. stirringit is stirred at 5° C. for 30 min
  2. customnitrogen being formed
  3. temperatureAfter cooling to room temperature
  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

来源与证据

ORD记录
ord-7fc91a129aeb4cb09cfa6ba7c7b4f71f
来源数据集
uspto-grants-1999_01
专利号
US05863864

关联笔记

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