反应详情

温度

0 °C

To a solution of glycolic acid (15 mg, 202 μmol) and DIPEA (35 mg, 270 μmol) in DMF (5 mL) is added HOBt (27 mg, 202 μmol) and EDC hydrochloride (39 mg, 202 μmol) at 0° C. The mixture is stirred for 15 min at 0° C. Then 2-{4-[5-(5-diethylaminomethyl-4-methyl-thiophen-2-yl)-[1,2,4]oxadiazol-3-yl]-phenyl}-ethylamine is added and stirring is continued for 1 h at 0° C. The reaction is quenched with water, diluted with sat. aq. NaHCO3 and the mixture is extracted three times with EA. The combined organic extracts are dried over MgSO4, filtered and concentrated. The crude product is purified on prep. TLC plates using DCM containing 10% of 7 N NH3 in methanol to give the title compound (4 mg) as a colourless oil; LC-MS: tR=0.69 min; [M+1]+=429.06.

1. stirringstirring
2. waitis continued for 1 h at 0° C
3. customThe reaction is quenched with water
4. additiondiluted with sat. aq. NaHCO3
5. extractionthe mixture is extracted three times with EA
6. dry with materialThe combined organic extracts are dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. customThe crude product is purified on prep