HRID421802
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of [6-(4-cyanophenyl)-5-(cyclopropylcarbonyl)-4-methyl-2-oxo-3-[3-(trifluoromethyl)phenyl]-3,6-dihydropyrimidin-1(2H)-yl]acetic acid (Example 31) (100 mg, 0.21 mmol), 1,3-dicyclohexylcarbodiimide (41.5 mg, 0.23 mmol), 4-cyanobenzene-1-sulfonamide (41.5 mg, 0.23 mmol) and 4-dimethylaminopyridine (28 mg, 0.23 mmol) in dichloromethane (4 ml) is stirred for 48 hours. The product is extracted with dichloromethane, washed with 2 N hydrochloric acid and brine, dried over anhydrous magnesium sulfate, filtered and concentrated. The residue is purified by preparative HPLC (RP18 column; eluent: acetonitrile/water 10:90→90:10).
WORKUP
后处理
- extractionThe product is extracted with dichloromethane
- washwashed with 2 N hydrochloric acid and brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe residue is purified by preparative HPLC (RP18 column; eluent: acetonitrile/water 10:90→90:10)