反应详情

温度

100 °C

To a solution of 24 in acetic acid (540 mL) was added sodium acetate (44.3 g, 540 mmol) and thiourea (28.8 g, 378 mmol). The reaction mixture was stirred with a mechanical stirrer at 100° C. for 3 h. The reaction mixture was partially concentrated in vacuo. EtOAc was added (500 mL). The mixture was made basic with 1 M NaOH, and the layers were separated. The aqueous layer was extracted with EtOAc (2×300 mL). The combined organic layers were dried, filtered, and concentrated in vacuo to give 49.3 g of 25, which was taken on without further purification. LCMS-ESI+: calc'd for C8H11N2OS: 183.1 (M+H+); Found: 183.1 (M+H+).

1. concentrationThe reaction mixture was partially concentrated in vacuo
2. additionEtOAc was added (500 mL)
3. customthe layers were separated
4. extractionThe aqueous layer was extracted with EtOAc (2×300 mL)
5. customThe combined organic layers were dried
6. filtrationfiltered
7. concentrationconcentrated in vacuo