Reaktion #429817

Reaktionsgleichung

3-hydroxypropylmercaptan

NaH

4-chloro-2,3-dimethylpyridine-N-oxide

→

2,3-Dimethyl-4-(3-hydroxypropylthio)pyridine-N-oxide

Lösungsmittel

N-methylpyrrolidone

NMP

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeare metered in in the course of 20 min
2. 2
   workup.STIRRINGthe mixture is stirred again for 30 min until the evolution of gas
3. 3
   workup.STIRRINGthe reaction mixture is stirred for 1 h at room tempera- ture
4. 4
   workup.WAITfor 1 h at 70° C.
5. 5
   Sonstigeadditionally for 1 h
6. 6
   Sonstigeat 100° C.

Vorschrift

6 g (60%) NaH are added in portions to 50 ml of dry N-methylpyrrolidone (NMP), the mixture is stirred for 15 min, 9.5 g (0.11 mol) of 3-hydroxypropylmercaptan are metered in in the course of 20 min and the mixture is stirred again for 30 min until the evolution of gas has ended. A solution of 14.4 g (0.1 mol) of 4-chloro-2,3-dimethylpyridine-N-oxide in 100 ml of NMP is then added dropwise in the course of 20 min, and the reaction mixture is stirred for 1 h at room tempera- ture, then for 1 h at 70° C. and after this additionally for 1 h at 100° C.

Quelle