反应详情

2-(2-Hydroxyethyl)-5-(4-acetamidobenzenesulfonyl)-1,5-benzothiazepine as prepared in Example 24 was dissolved in a 10% HCl/MeOH (100 ml) solution and stirred at reflux for 2½ hours. The mixture was cooled and a saturated NaHCO3 solution 160 ml) was added. The methanol was removed under reduced pressure and the aqueous mixture extracted with EtOAc (2×80 ml). The combined EtOAc extracts were dried (MgSO4), filtered and evaporated in vacuo to give the desired product as a solid (2.4 g,92%) m.p. 145-148° C. 1H NMR (300 MHz, DMSOd6) 6 7.50( d, J=7 Hz, 1H); 7.41 (d, J=8.6 Hz, 2H); 7.33-7.19 (m, 3H); 6.59 (d, J=8.6 Hz, 2H); 6.05(s, 2H) 4.51 (t, J=5 Hz, 1H); 3.45-3.35 (m, 4H); 2.96 (m, 1H), 2.07(m, 1H); 1.81(m, 1H); 1.49(m, 2H) . m/z (MH+) 365.

1. temperatureat reflux for 2½ hours
2. temperatureThe mixture was cooled
3. customThe methanol was removed under reduced pressure
4. extractionthe aqueous mixture extracted with EtOAc (2×80 ml)
5. dry with materialThe combined EtOAc extracts were dried (MgSO4)
6. filtrationfiltered
7. customevaporated in vacuo