反应详情

To the mixture containing (E)-3-(3,5-dichlorophenyl)-1-(4-(2-(methylamino)ethyl)piperidin-1-yl)prop-2-en-1-one (step 5) (118 mg, 0.346 mmol) and 2-oxo-2,3-dihydrooxazole-5-carboxylic acid (step 7) (2.59 ml, 0.2M solution in DMF, 0.519 mmol) and DIPEA (0.483 ml, 2.77 mmol) in DMF (3.458 ml) was added T3P® (50% solution in EtOAc) (2.421 ml, 4.149 mmol). The reaction mixture was stirred at RT for 1 h. Water was added to quench the excess T3P® and the solvent was removed under reduced pressure. The residue was passed through an Isolute SCX-2 cartridge (10 g) and washed with excess MeOH. The solvent was removed under reduced pressure to afford a yellow oil which was dried using a high vacuum oven. The crude material was purified using preparative HPLC with water (+0.1% TFA) and acetonitrile (+0.1% TFA) and the product fractions were concentrated under high vacuum to afford the title compound as a clear film;

1. customto quench the excess T3P®
2. customthe solvent was removed under reduced pressure
3. washwashed with excess MeOH
4. customThe solvent was removed under reduced pressure
5. customto afford a yellow oil which
6. customwas dried
7. customThe crude material was purified
8. concentrationthe product fractions were concentrated under high vacuum