反应详情

温度

40 °C

A suspension of compound of Example 1a (1.0 eq) in DCM (approx 3.4 vol) is treated with thionyl chloride (1.0-1.2 eq, for example 1.1 eq) and catalytic amount (0.011 eq) of DMF and the mixture is stirred for 16 h at 40° C. DCM is distilled off (approx 2.7 vol) and the residue is diluted with THF (approx 1.8 vol). The excess of thionylchloride is distilled off with THF/DCM and the residue after distillation is cooled to 10° C.

1. distillationDCM is distilled off (approx 2.7 vol)
2. additionthe residue is diluted with THF (approx 1.8 vol)
3. distillationThe excess of thionylchloride is distilled off with THF/DCM
4. distillationthe residue after distillation
5. temperatureis cooled to 10° C.