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
0.26 cm3 of butyryl chloride is added to 500 mg of 5-(trifluoromethyl)-1H-indazole-3-amine, prepared according to patent U.S. Pat. No. 3,133,081, in 15 cm3 of pyridine, and cooled to about 5° C. The reaction medium is allowed to return to about 19° C. over 12 hours. The reaction medium is evaporated under reduced pressure (2 kPa; 50° C.). The residue is taken up in 15 cm3 of ethyl acetate and 15 cm3 of distilled water. The organic phase is dried over magnesium sulphate, filtered through a sinter funnel and then evaporated under reduced pressure (2 kPa; 50° C.). The residue is taken up in 15 cm3 of dichloromethane, filtered and dried under reduced pressure (90 Pa; 50° C.) to give 390 mg of N-[5-(trifluoromethyl)-1H-indazol-3-yl]butanamide in the form of an off-white solid melting at 230° C.
WORKUP
后处理
- customprepared
- customThe reaction medium is evaporated under reduced pressure (2 kPa; 50° C.)
- dry with materialThe organic phase is dried over magnesium sulphate
- filtrationfiltered through a sinter funnel
- customevaporated under reduced pressure (2 kPa; 50° C.)
- filtrationfiltered
- customdried under reduced pressure (90 Pa; 50° C.)