反应详情

16% aqueous TiCl3 (2 mL) was added to a solution of Example 25 (0.10 g, 0.23 mmol) in AcOH/H2O (2 mL, 1:1). After stirring for 15 min, the reaction was made basic with 1N NaOH and NaHCO3 and stirred for 30 min. The layers were separated and the aqueous layer was reextracted with CHCl3 /CH3OH (9/1). The combined organic layers were dried over MgSO4, filtered and concentrated to afford 0.92 g. (73%) of Example 26. A 20 mg. sample of this material was treated with 1M HCl in ether (2 mL). A light yellow solid was formed which was triturated several times with ether and dried under vacuum to afford Example 26 (23 mg.) as a light yellow solid. (Example 26 is also Compound G of Example 22.)

1. stirringstirred for 30 min
2. customThe layers were separated
3. dry with materialThe combined organic layers were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customto afford 0.92 g
7. customA light yellow solid was formed which
8. customwas triturated several times with ether
9. customdried under vacuum
10. customto afford Example 26 (23 mg.) as a light yellow solid