反应详情

The title compound was prepared in accordance with the general method described in Example 12(a) by using 1-(3-isopropyl-isoxazol-5-yl)methylamine (0.85 g, 6.06 mmol), benzoyl isothiocyanate (0.90 mL, 6.67 mmol) and ammonia in methanol (7 N, 30 mL) with the exception that the reaction time for amine with benzoyl isothiocyanate was 12 h and the reaction mixture in ammonia was stirred o.n. Work-up was done by concentrating the reaction mixture in vacuo and adding ethyl acetate (15 mL) and water (15 mL). The is organic layer was separated, dried over sodium sulfate, filtered and concentrated. The residue was triturated with diethyl ether (10 mL) and the solid was removed by filtration. The filtrate was concentrated in vacuo to give the title compound (1.11 g, 91% yield), which was used in the next step without further purification. MS (ESI) m/z 200 (M+1).

1. customThe title compound was prepared in accordance with the general method
2. concentrationby concentrating the reaction mixture in vacuo
3. additionadding ethyl acetate (15 mL) and water (15 mL)
4. customThe is organic layer was separated
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was triturated with diethyl ether (10 mL)
9. customthe solid was removed by filtration
10. concentrationThe filtrate was concentrated in vacuo