反应详情

温度

0 °C

A suspension of 0.080 g (0.24 mmol) of 5-(3-benzofuran-2-yl-phenyl)-1,4-dimethyl-1H-pyrazole-3-carboxylic acid (Example 16C]) in 1.5 ml of CH2Cl2 was treated at RT with 1 drops of DMF. 0.02 ml (0.29 mmol, 1.2 eq) of oxalyl chloride in 0.5 ml CH2Cl2 were added dropwise and stirring was continued for 1 h. The solution was evaporated, redissolved in 1 ml of CH2Cl2, cooled (0° C.) and treated with a solution of 0.041 g (0.24 mmol, 1 eq) of 4-(piperidine-4-yl)-morpholine and 0.07 ml (0.48 mmol, 2 eq) of triethylamine in 0.5 ml of CH2Cl2. The reaction was stirred for 3 h at this temperature, then partitioned three times between EtOAc and aqueous saturated NaHCO3, dried over Na2SO4 and evaporated to give 0.134 g (quant.) of the title compound as light yellow foam. MS: 485.3 (MH+).

1. customThe solution was evaporated
2. dissolutionredissolved in 1 ml of CH2Cl2
3. stirringThe reaction was stirred for 3 h at this temperature
4. custompartitioned three times between EtOAc and aqueous saturated NaHCO3
5. dry with materialdried over Na2SO4
6. customevaporated