反应详情

To a stirred suspension of 1-methyl-3-(1-methylethyl)-5-(methyloxy)-1H-indole-7-carboxylic acid (78 mg, 0.315 mmol), 3-(aminomethyl)-4,6-dimethyl-2(1H)-pyridinone hydrochloride (59.5 mg, 0.315 mmol), HOAt (64 mg, 0.473 mmol) in DMF (4 mL) was added EDC (121 mg, 0.631 mmol) and N-methylmorpholine (52 μL, 0.473 mmol). The reaction mixture was stirred for 18 hr at room temperature, after which time the contents were evaporated to near dryness. Water (˜5 mL) was added and the solids which precipitated out were isolated. The collected solid was dissolved in DCM/MeOH (4:1, 5 mL), dried over MgSO4, filtered, and concentrated in vacuo to a afford a creme colored solid. The solid was re-dissolved in DCM/MeOH (4:1, 5 mL) and washed with 6N NaOH (1 mL) and water (4 mL). The organic layer was concentrated in vacuo to afford a nearly white solid.

1. customafter which time the contents were evaporated
2. additionWater (˜5 mL) was added
3. customthe solids which precipitated out
4. customwere isolated
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo to
8. customa afford a creme colored solid
9. washwashed with 6N NaOH (1 mL) and water (4 mL)
10. concentrationThe organic layer was concentrated in vacuo
11. customto afford a nearly white solid