反应详情

To a solution of #168 (36.9 mg, 0.158 mmol, 1 eq.) and #114 (100 mg, 0.158 mmol, 1 eq.) in dichloromethane (3.6 mL) and N,N-dimethylformamide (0.8 mL), was added diisopropylethylamine (0.083 mL, 0.474 mmol, 3 eq.) followed by HATU (60.7 mg, 0.158 mmol, 1 eq.). The reaction was allowed to stir at room temperature for 18 hours, diluted with ethyl acetate (25 mL), washed with water (1×), 10% citric acid (1×) and brine (1×). The organic layer was dried over sodium sulfate, filtered, and the filtrate concentrated in vacuo to give crude #216 (220 mg, 164% of theory) which was used in next step without further purification. HPLC (protocol Q): m/z 848.6 [M+H+], retention time=2.10 minutes.

1. washwashed with water (1×), 10% citric acid (1×) and brine (1×)
2. dry with materialThe organic layer was dried over sodium sulfate
3. filtrationfiltered
4. concentrationthe filtrate concentrated in vacuo
5. customto give crude #216 (220 mg, 164% of theory) which
6. customwas used in next step without further purification