Reaktion #430930

Reaktionsgleichung

4-methyl-5-nitro-1,1,3-trioxo-2,3-dihydro-1λ6 benz[d]isothiazole

Hydrogen

→

4-Methyl-5-amino-1,1,3-trioxo-2,3-dihydro-1λ6 benz[d]isothiazole

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstige9 l of H2 are absorbed in the course of 4.5 hours
2. 2
   TemperaturAfter cooling to 25° C.
3. 3
   Filtrationthe catalyst is filtered off
4. 4
   Einengenthe filtrate is concentrated to a volume of 200 ml (on a Rotavapor) and
5. 5
   FiltrationThe deposited precipitate is filtered off with suction
6. 6
   Waschenwashed with water
7. 7
   Sonstigedried under reduced pressure at 50° C
8. 8
   Sonstige23.4 g (0.11 mol=85% of theory) of a white solid of m.p.: 272°-273° C. are obtained

Vorschrift

33.6 g (0.13 mol) of 4-methyl-5-nitro-1,1,3-trioxo-2,3-dihydro-1λ6 benz[d]isothiazole are dissolved in 1.2 l of water with warming to 45° C. and 5 g of Pd/C (10 percent 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 (on a Rotavapor) 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.

Quelle