Acetyl chloride → HCID 58613284, compound

Participants

Reaction Steps

To a solution of 4-chloro-6-((3S,5R)-3,5-dimethylpiperazin-1-yl)pyrimidine(1, 10.29 g, 45.4 mmol) and DIEA (8.80 g, 68.1 mmol. 1.50 equiv.) in 100 ml DCM was added acetyl chloride (4.03 ml, 56.7 mmol, 1.25 equiv.) at room temperature portionwise over 10 min. The reaction was stirred at room temperature for another 30 min. Aqueous NaHCO3 was added to the reaction and the organic layer was washed with NahCO3 (100 ml×2) followed by saturated aqueous NaCl solution. The organic layer was dried over Organic layer was dried over NacSO4. Removal of solvent left a yellow oil. This oily material was triturated in diethyl ether to afford a white solid. The solid was collected by filtration and the washed with diethyl ether again. The solid was dried under vacuum and was weighted at 11.95 g. The yield is 98.2%. LC/MS (M+1=269.1).

Provenance & Evidence