반응 #58693

반응 방정식

L-tartaric acid

1-(2-fluoro-phenyl)-3-(piperidin-4-yloxy)-1H-indazole hydrochloride

Sodium carbonate

ether

→

L-tartrate salt—1-(2-fluoro-phenyl)-3-(piperidin-4-yloxy)-1H-indazole L-tartrate

수율 124.9%

용매

water

tetrahydrofuran

water

반응 조건

후처리

1. 1
   기타formed
2. 2
   workup.STIRRINGThe mixture was shaken
3. 3
   기타the layers were separated
4. 4
   추출The aqueous layer was extracted with ether (100 ml)
5. 5
   건조The combined organic layers were dried over magnesium sulfate
6. 6
   농축concentrated in vacuo to a gum (8.0 g, 99% crude)
7. 7
   workup.ADDITIONTo this gum was added
8. 8
   workup.STIRRINGThe mixture was stirred for ˜2 minutes when a complete solution
9. 9
   기타formed
10. 10
    workup.STIRRINGStirring
11. 11
    workup.WAITwas continued and after ˜2 minutes
12. 12
    기타solid began precipitating
13. 13
    workup.STIRRINGThe suspension was stirred at 0° C. for 3 hours
14. 14
    여과filtered
15. 15
    세척The solid was rinsed with water (15 ml)
16. 16
    기타pressed dry under suction
17. 17
    기타Further drying in vacuo at 50° C. for 16 hours

실험 절차

A mixture of 1-(2-fluoro-phenyl)-3-(piperidin-4-yloxy)-1H-indazole hydrochloride (9.0 g, 0.026 moles) in tetrahydrofuran (20 ml) and water (100 ml) was stirred at room temperature for 0.5 hour as a solution formed. Sodium carbonate (15 g, 0.142 moles) was added portion-wise over a 5-minute period, followed by ether (150 ml). The mixture was shaken and the layers were separated. The aqueous layer was extracted with ether (100 ml). The combined organic layers were dried over magnesium sulfate and concentrated in vacuo to a gum (8.0 g, 99% crude). To this gum was added, all at once, a solution of L-tartaric acid (4.0 g, 0.0267 mol) in water (80 ml). The mixture was stirred for ˜2 minutes when a complete solution formed. Stirring was continued and after ˜2 minutes solid began precipitating. The suspension was stirred at 0° C. for 3 hours and filtered. The solid was rinsed with water (15 ml) and pressed dry under suction. Further drying in vacuo at 50° C. for 16 hours provided 10.2 g (85.5%) of the L-tartrate salt—1-(2-fluoro-phenyl)-3-(piperidin-4-yloxy)-1H-indazole L-tartrate.

출처