反应详情

A mixture of 2-bromo-3-methyl-benzoic acid (62, 0.016 g, 0.075 mmol), resin-bound carbodiimide (0.078 g, 0.15 mmol) and HOBT (0.012 g, 0.085 mmol) in DCM:DMF (1 mL, 10:1) was shaken for 18 h. A solution of 42b (0.022 g, 0.05 mmol) and DIPEA (0.03 mL, 0.17 mmol) and DCM (1 mL) was added. Shaking was continued for 24 h, the resin filtered and washed with DMF (1 mL) and twice with DCM (1 mL). The reaction mixture was concentrated in vacuo and purified by reverse phase HPLC to afford II-244: ms (ES+) m/z 644 (M+H)+.

1. filtrationthe resin filtered
2. washwashed with DMF (1 mL) and twice with DCM (1 mL)
3. concentrationThe reaction mixture was concentrated in vacuo
4. custompurified by reverse phase HPLC
5. customto afford II-244: ms (ES+) m/z 644 (M+H)+