反应详情

A mixture of ethyl (2S)-2-(tert-butoxy)-2-{4,24-dimethyl-11,23-dioxa-1,5,7,8-tetraazapentacyclo[22.2.2.16,9.113,17.02,7]triaconta-2,4,6(30),8,13(29),14,16-heptaen-3-yl}acetate (20 mg, 0.034 mmol) and NaOH (0.169 mL, 0.169 mmol) in EtOH (2 mL) was refluxed for 2 h. It was then filtered and purified by preparative HPLC to isolate (2S)-2-(tert-butoxy)-2-{4,24-dimethyl-11,23-dioxa-1,5,7,8-tetraazapentacyclo[22.2.2.16,9.113,17.02,7]triaconta-2,4,6(30),8,13(29),14,16-heptaen-3-yl}acetic acid (10 mg, 0.017 mmol, 51.4% yield) as a white solid. 1H NMR (500 MHz, DMSO-d6) δ 7.34-7.27 (m, 1H), 7.22 (s, 1H), 7.16 (d, J=7.3 Hz, 2H), 6.50 (s, 1H), 5.62 (s, 1H), 4.62-4.40 (m, 4H), 4.17 (t, J=12.5 Hz, 1H), 3.65-3.56 (m, 1H), 3.38-3.23 (m, 2H), 2.77 (d, J=11.4 Hz, 1H), 2.74-2.66 (m, 1H), 2.59-2.53 (m, 1H), 2.50 (br. s., 4H), 1.91 (d, J=12.5 Hz, 1H), 1.84-1.75 (m, 1H), 1.75-1.62 (m, 3H), 1.58-1.44 (m, 3H), 1.43-1.33 (m, 2H), 1.17 (s, 3H), 1.14 (s, 9H). LCMS (M+1)=565.3.

1. temperaturewas refluxed for 2 h
2. filtrationIt was then filtered
3. custompurified by preparative HPLC