반응 #2157072

반응 방정식

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

용매

toluene

triethylamine

water

반응 조건

후처리

1. 1
   기타To 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
   기타After separating into the organic layer
6. 6
   기타the aqueous layer, the aqueous layer is removed
7. 7
   세척the organic layer is washed once with 220.0 g of 5% hydrochloric acid
8. 8
   세척washed once with 220.0 g of water
9. 9
   농축The organic layer is concentrated

실험 절차

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)).

출처