反应详情

(R,R)-2-aminocyclopentanol×HCl (155 mg) is added to a suspension of NaH (135.2 mg) in dioxane (0.75 mL) and stirred for 30 min at RT. Then 4-(4-chloro-5-trifluoromethyl-pyrimidin-2-ylamino)-3-methoxy-N-(1-methyl-piperidin-4-yl)-benzamide (250 mg) is added. After 18 h, H2O (50 mL) is added. The precipitate formed is filtered off, washed with H2O, dissolved in CH2Cl2 and extracted with aqueous KHSO4 solution (10%). The aqueous phase is made basic again with K2CO3 and extracted with CH2Cl2. The organic phase is dried on magnesium sulphate, filtered to remove the desiccant and the solvent is eliminated in vacuo.

1. waitAfter 18 h
2. customThe precipitate formed
3. filtrationis filtered off
4. washwashed with H2O
5. dissolutiondissolved in CH2Cl2
6. extractionextracted with aqueous KHSO4 solution (10%)
7. extractionextracted with CH2Cl2
8. customThe organic phase is dried on magnesium sulphate
9. filtrationfiltered
10. customto remove the desiccant