反应详情

温度

110 °C

A solution of Intermediate 105a (194 mg, 0.635 mmol) in toluene (13 mL) was treated with HCl (37%, 3.5 mL) and heated at 110° C. for 1.5 h. After cooling to RT, the reaction mixture was diluted with water and extracted with toluene (×3). The aqueous layer was cooled to 0° C., neutralised with 5N NaOH and extracted with DCM (×3). The combined organic layers were dried (MgSO4) and concentrated in vacuo to afford the title compound (78 mg, 86%) as a silver/green solid. LCMS (Method 4): Rt 0.29 min, m/z 142 [MH+].

1. temperatureAfter cooling to RT
2. extractionextracted with toluene (×3)
3. temperatureThe aqueous layer was cooled to 0° C.
4. extractionextracted with DCM (×3)
5. dry with materialThe combined organic layers were dried (MgSO4)
6. concentrationconcentrated in vacuo