反应详情

温度

20 °C

To a solution of Intermediate 119 1-[2-(3,5-dimethyl-phenyl)-acetyl]-2-methyl-azetidine-2-carboxylic acid (1 eq.) in either DCM, THF or DMF was added HOBt (1.1 eq.), EDC.HCl (1.5 eq.), TEA (3 eq.) and methyl-(4-methyl benzyl)-amine (1.5 eq.). The reaction was stirred at 20° C. for 15 h, then the crude was concentrated under reduced pressure and partitioned between a saturated aqueous solution of NaHCO3 and EtOAc. The aqueous layer was extracted three times with EtOAc. The organic layers were combined, washed with water then with brine, dried over MgSO4, filtered and concentrated under reduced pressure. The crude was purified by chromatography on silica gel (elution with DCM/MeOH: 100/0 to 99/1) to afford 1-[2-(3,5-dimethyl-phenyl)-acetyl]-2-methyl-azetidine-2-carboxylic acid methyl-(4-methyl-benzyl)-amide.

1. concentrationthe crude was concentrated under reduced pressure
2. custompartitioned between a saturated aqueous solution of NaHCO3 and EtOAc
3. extractionThe aqueous layer was extracted three times with EtOAc
4. washwashed with water
5. dry with materialwith brine, dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe crude was purified by chromatography on silica gel (elution with DCM/MeOH: 100/0 to 99/1)