Reaktion #2157072

Reaktionsgleichung

3,3-dimethylpyrrolidine

4,5,6-trifluoropyrimidine

potassium carbonate

2-butyn-1-ol

→

4-(2-butynyloxy)-5-fluoro-6-(3,3-dimethylpyrrolidin-1-yl)pyrimidine

Lösungsmittel

toluene

triethylamine

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a mixture obtained
2. 2
   workup.ADDITIONis added dropwise at 25 to 30° C. over one hour
3. 3
   workup.STIRRINGby stirring
4. 4
   workup.STIRRINGafter the mixture is stirred at 30° C.
5. 5
   SonstigeAfter separating into the organic layer
6. 6
   Sonstigethe aqueous layer, the aqueous layer is removed
7. 7
   Waschenthe organic layer is washed once with 220.0 g of 5% hydrochloric acid
8. 8
   Waschenwashed once with 220.0 g of water
9. 9
   EinengenThe organic layer is concentrated

Vorschrift

To a mixture obtained by adding 110.0 g of 4,5,6-trifluoropyrimidine, 114.6 g of potassium carbonate and 16.6 g of triethylamine to 220.0 g of toluene, 60.4 g of 2-butyn-1-ol is added dropwise at 25 to 30° C. over one hour, followed by stirring at 30° C. Then, 220.0 g of water is added dropwise into the reaction mixture, followed by stirring. Then, 85.4 g of 3,3-dimethylpyrrolidine is added dropwise and, after the mixture is stirred at 30° C., the reaction mixture is allowed to stand. After separating into the organic layer and the aqueous layer, the aqueous layer is removed and the organic layer is washed once with 220.0 g of 5% hydrochloric acid and then washed once with 220.0 g of water. The organic layer is concentrated to obtain 4-(2-butynyloxy)-5-fluoro-6-(3,3-dimethylpyrrolidin-1-yl)pyrimidine (hereinafter referred to as the present compound (1)).

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