反应详情

The procedure of Example 1 was carried out using 2-amino-2'-fluorobenzophenone (1.26 gm, 5.86 mmol), N-Boc-β-(2-thienyl)-DL-alanine (1.75 gm, 6.45 mmol), and DCC (6.45 ml of 1.0M solution in CH2Cl2) in CH2Cl2 (25 ml). Filtration, concentration in vacuo and flash chromatography (silica gel, 1% (v/v) Et2O in CH2Cl2) gave a white foam which was deprotected and cyclized by the procedure of Example 2. After stirring 3 days, the mixture was evaporated in vacuo, treated with H2O (50 ml) and extracted with EtOAc (2×100 ml). The combined organic extracts were washed with brine (50 ml), dried over MgSO4, filtered, and evaporated to dryness in vacuo. The resulting foam was crystallized from Et2O to give the title compound as a white solid. The solid was dried in vacuo at 65° C.: (m.p. 189°-91° C.).

1. filtrationFiltration, concentration in vacuo and flash chromatography (silica gel, 1% (v/v) Et2O in CH2Cl2)
2. customgave a white foam which
3. customthe mixture was evaporated in vacuo
4. additiontreated with H2O (50 ml)
5. extractionextracted with EtOAc (2×100 ml)
6. washThe combined organic extracts were washed with brine (50 ml)
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. customevaporated to dryness in vacuo
10. customThe resulting foam was crystallized from Et2O