反応 #905

反応方程式

4-methyl-5-nitrosaccharin

Hydrogen

→

4-Methyl-5-aminosaccharin

溶媒

water

反応条件

後処理

1. 1
   その他9 l of H2 are absorbed in the course of 4.5 hours
2. 2
   温度After cooling to 25° C.
3. 3
   ろ過the catalyst is filtered off
4. 4
   濃縮the filtrate is concentrated to a volume of 200 ml
5. 5
   ろ過The deposited precipitate is filtered 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23.4 g (0.11 mol=85% of theory) of a white solid of m.p.: 272°-273° C. are obtained

実験手順

33.6 g (0.13 mol) of 4-methyl-5-nitrosaccharin are dissolved in 1.2 l of water with warming to 45° C. and 5 g of Pd/C (10% on active carbon) are added. Hydrogen gas is then passed in with vigorous stirring (pressureless hydrogenation). 9 l of H2 are absorbed in the course of 4.5 hours. After cooling to 25° C., the catalyst is filtered off, and the filtrate is concentrated to a volume of 200 ml and then acidified to pH 1. The deposited precipitate is filtered off with suction, washed with water and dried under reduced pressure at 50° C. 23.4 g (0.11 mol=85% of theory) of a white solid of m.p.: 272°-273° C. are obtained.

出典