反应详情

温度

10 °C

A suspension of compound of Example 1a (1.0 eq) in DCM (approx 4.5 vol) is treated with thionyl chloride (1.0-1.2 eq, for example 1.1 eq) and catalytic amount (0.0055 eq) of DMF and the mixture is stirred for 16 h at reflux. Unreacted thionylchloride is distilled off with DCM and the residue after distillation is diluted with THF (approx 1.8 vol) and cooled to 10° C.

1. temperatureat reflux
2. distillationUnreacted thionylchloride is distilled off with DCM
3. distillationthe residue after distillation
4. additionis diluted with THF (approx 1.8 vol)