反应详情

To a solution of 1-(trifluoromethyl)cyclopropanecarboxylic acid (0.159 g, 1.03 mmol) in DCM was added oxalyl chloride (0.081 ml, 0.928 mmol) and catalytic DMF. Once gas evolution ceased, this crude reaction mixture was added portion-wise to a suspension of 2-(1-(2,3-difluorobenzyl)-5-(isoxazol-3-yl)-1H-pyrazol-3-yl)pyrimidine-4,5-diamine hydrochloride (Compound 8, 40 mg, 0.100 mmol) in dichloromethane/pyridine (2 ml/2 ml) until complete consumption of starting material was observed by LS/MS. After an ammonium chloride (saturated aqueous) and dichloromethane workup, column chromatography (0-10% MeOH/DCM) provided the desired product as an off-white solid (36%).

1. customthis crude reaction mixture
2. additionwas added portion-wise
3. customuntil complete consumption of starting material