反应详情

To a mixture of 2-(2-hydroxyethyl)-1,5-benzothiazepine as prepared in Example 2 (3 g, 14.4 mM) in pyridine (30 ml) was slowly added N-acetylsulfanilyl chloride (6.7 g, 28.7 mM). The resulting mixture was stirred at room temperature for 16 hours and the excess pyridine was removed under reduced pressure. The residual semi-solid was diluted with H2O (80 ml) and extracted with CH2Cl2 (2×80 ml). The combined methylene chloride extracts were dried (MgSO4), filtered and evaporated in vacuo to give a crude oil. Flash column chromatography (EM silica gel 60; 2% MeOH in CH2Cl2) gave the desired product as a white solid (2.9 g, 50%). m/z (MH+)407

1. customthe excess pyridine was removed under reduced pressure
2. additionThe residual semi-solid was diluted with H2O (80 ml)
3. extractionextracted with CH2Cl2 (2×80 ml)
4. dry with materialThe combined methylene chloride extracts were dried (MgSO4)
5. filtrationfiltered
6. customevaporated in vacuo
7. customto give a crude oil