反应详情

[(2S)-8-methyl-2,3-dihydro[1,4]dioxino[2,3-f]quinolin-2-yl]methylamine hydrochloride (360 mg, 1.35 mmol) and compound I were suspended in anhydrous tetrahydrofuran (THF) containing triethylamine (1.8 mL) and HOBT (54 mg) with stirring for 15 min. The coupling reagent, DCC (300 mg) was added and stirring was continued overnight. The reaction mixture was filtered and the filtrate was diluted with water and extracted with ether. The ether layers were combined, dried (MgSO4), and evaporated under reduced pressure to give a residue which was purified by flash chromatography on silica gel eluting with 1-2% methanol in methylene chloride to give the intermediate II (240 mg) as a white solid. mp 262-267° C.; MS (ES) m/z 444.3.

1. stirringstirring
2. waitwas continued overnight
3. filtrationThe reaction mixture was filtered
4. additionthe filtrate was diluted with water
5. extractionextracted with ether
6. dry with materialdried (MgSO4)
7. customevaporated under reduced pressure
8. customto give a residue which
9. customwas purified by flash chromatography on silica gel eluting with 1-2% methanol in methylene chloride