反应详情

200 mg of 2-(5-cyclopropyl-4-methyl-1H-pyrazol-3-yl)-5-methoxy-N-(pyridin-4-yl)pyrimidin-4-amine 1-16-1 (0.62 mmol, 1.0 eq.), 184.86 mg of methyl 3-(bromomethyl)-2,4-dichlorobenzoate (0.62 mmol, 1.0 eq.) and 31.0 mg of 60% sodium hydride in paraffin oil were suspended in 6.3 mL of dry THF and stirred for 20 hours at rt. The reaction mixture was partitioned between water and DCM/propan-2-ol 4:1. The separated aqueous layer was extracted three times with DCM/propan-2-ol 4:1. The combined organic layers were dried over sodium sulfate and concentrated in vacuo. The purification by flash chromatography and preparative HPLC of the residue provided 37.5 mg (0.07 mmol, 11%) of analytically pure target compound.

1. customThe reaction mixture was partitioned between water and DCM/propan-2-ol 4:1
2. extractionThe separated aqueous layer was extracted three times with DCM/propan-2-ol 4:1
3. dry with materialThe combined organic layers were dried over sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe purification by flash chromatography and preparative HPLC of the residue
6. customprovided 37.5 mg (0.07 mmol, 11%) of analytically pure target compound