反应详情

2.0 g of 4-(5-chloro-2-pyrimidinyloxy)-3-methylaniline and 1.3 ml of triethylamine were dissolved in 20 ml of tetrahydrofuran, and 1.12 ml of valeryl chloride was dropwise added thereto under cooling with ice. The mixture was reacted at room temperature for 40 minutes under stirring. After completion of the reaction, the reaction product was poured into water and extracted with ethyl acetate. The extract layer was washed with a saturated aqueous solution of sodium chloride and dried over Glauber's salt. Then, ethyl acetate was distilled off to obtain 2.8 g of N-[4-(5-chloro-2-pyrimidinyloxy)-3-methylphenyl]valeramide (Intermediate Compound No. 13) (melting point: 146°-150° C.)

1. temperatureunder cooling with ice
2. customThe mixture was reacted at room temperature for 40 minutes
3. customAfter completion of the reaction
4. extractionextracted with ethyl acetate
5. washThe extract layer was washed with a saturated aqueous solution of sodium chloride
6. dry with materialdried over Glauber's salt
7. distillationThen, ethyl acetate was distilled off