反応 #906

反応方程式

HCl

potassium iodide

4-methyl-5-aminosaccharin

sodium nitrite

→

iodine

4-Methyl-5-iodosaccharin

溶媒

water

acetic acid

water

反応条件

後処理

1. 1
   workup.STIRRINGit is stirred at 5° C. for 30 min
2. 2
   その他nitrogen being formed
3. 3
   温度After cooling to room temperature
4. 4
   その他the deposited product is isolated
5. 5
   ろ過by filtering off with suction
6. 6
   洗浄washed with water
7. 7
   その他dried under reduced pressure at 50° C
8. 8
   その他32.5 g (0.1 mol=91% of theory) of a solid of m.p.: 257°-258° C. are obtained

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 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%).

出典