反应详情

温度

50 °C

Sodium (2-methylthiazol-4-yl)methanesulfonate, 40, (357 mg, 1.66 mmol) is dissolved in phosphorous oxychloride (6 mL) and is treated with phosphorous pentachloride (345 mg, 1.66 mmol). The reaction mixture is stirred at 50° C. for 3 hours, then allowed to cool to room temperature. The solvent is removed under reduced pressure and the residue is re-dissolved in CH2Cl2 (40 mL) and is washed with sat. NaHCO3 and brine. The organic layer is dried over MgSO4, filtered, and the solvent removed in vacuo to afford 0.095 g of the desired product as a brown oil. LC/MS ESI+ 211 (M+1). Intermediates are obtained in sufficient purity to be carried forward according to Scheme IX without the need for further purification.

1. temperatureto cool to room temperature
2. customThe solvent is removed under reduced pressure
3. dissolutionthe residue is re-dissolved in CH2Cl2 (40 mL)
4. washis washed with sat. NaHCO3 and brine
5. dry with materialThe organic layer is dried over MgSO4
6. filtrationfiltered
7. customthe solvent removed in vacuo