反应详情

温度

0 °C

The final product from Example 16 (25 mg) was placed in a Syn 10 (Radleys) reaction tube together with a magnetic stirrer, and the material was dissolved in methanol by the addition of one aliquot (1 mL) of methanol preheated to 50° C. with stirring. A further 5 mg of methanol was added to the reaction tube to ensure a super-saturated solution was produced on cooling. When the majority of the solid had dissolved, the resultant solution was filtered through a Pall 0.45 μm PTFE Acrodisc CR13 filter into a second tube at 50° C. in the Syn 10. The tube was then cooled to 0° C. at a rate of 3° C./min and held at 0° C. until the material had crystallized. The samples were filtered off, dried by suction then by standing in ambient conditions. The solids were carefully removed from the filter paper and examined by XRPD.

1. custompreheated to 50° C.
2. customwas produced
3. temperatureon cooling
4. dissolutionWhen the majority of the solid had dissolved
5. filtrationthe resultant solution was filtered through a Pall 0.45 μm PTFE Acrodisc CR13
6. filtrationfilter into a second tube at 50° C. in the Syn 10
7. customheld at 0° C. until the material
8. customhad crystallized
9. filtrationThe samples were filtered off
10. customdried by suction
11. customThe solids were carefully removed from the filter paper