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With 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; N-ethyl-N,N-diisopropylamine; In dichloromethane; at 20℃; for 18.0h;
Ste D; To a solution of 2,3,6-trifluorophenyl acetic acid (5.5 g, 29 mmol) and the intermediate from step C (5.0 g, 34 mmol) in DCM (20 ml) was added EDCI (7.9 g, 41.2 mmol) followed by DIEA (17.99 ml, 103 mmol). After stirring the reaction at room temperature for 18 hours, it was diluted with DCM (100 mL), and washed with water (2X). The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated to give a brown solid, LC-MS: m/z=282 (M+l); rt=0.6 min (Method C).
With 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; N-ethyl-N,N-diisopropylamine; In dichloromethane; at 18 - 25℃; for 18.0h;
To a solution of 2,3,6-trifluorophenyl acetic acid (5.5 g, 29 mmol) and the intermediate from Step C (5.0 g, 34 mmol) in DCM (20 mL) was added EDC (7.9 g, 41.2 mmol) followed by DIEA (17.99 mL, 103 mmol). After stirring the reaction at room temperature for 18 hours, it was diluted with DCM (100 mL), and washed with water (2X). The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated to give a brown solid. LC3 rt = 0.6 min, m/z = 282 (M+H).
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