反应详情

To a mixture of 16-(3-(4-(diethyl amino)-2-(4-(3-(trifluoromethyl)benzylcarbamoyl)pyridin-2-yl)phenylcarbamoyl)phenyl)-4,7,10,13-tetraoxahexadecan-1-oic acid (292 mg, 0.36 mmol), tert-butyl piperazine-1-carboxylate (75 mg, 0.40 mmol) and DIPEA (142 mg, 1.1 mmol) in DMF (3 mL) was added HATU (160 mg, 0.42 mmol). After 30 minutes, the solvent was removed under vacuum and the residue was dissolved in DCM (50 mL). This was washed with water (4×25 mL), dried (Na2SO4) and concentrated. The resulting oil was dissolved in DCM (2 mL) and TFA (2 mL) was added dropwise. After 30 minutes, the solvents were removed under vacuum. The residue was dissolved in 50% ACN/water (30 mL) and freeze dried to give the title compound (560 mg) as a TFA salt.

1. customthe solvent was removed under vacuum
2. dissolutionthe residue was dissolved in DCM (50 mL)
3. washThis was washed with water (4×25 mL)
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated
6. dissolutionThe resulting oil was dissolved in DCM (2 mL)
7. additionTFA (2 mL) was added dropwise
8. waitAfter 30 minutes
9. customthe solvents were removed under vacuum
10. dissolutionThe residue was dissolved in 50% ACN/water (30 mL)
11. customfreeze dried