Hydrochloric Acid → (3,5-Dibromo-4-hydroxy-phenyl)-[7-(4-trifluoromethyl-phenyl)-2,3-dihydro-pyrido[2,3-b][1,4]oxazin-1-yl]-methanone

In a 10 ml flask, (3,5-dibromo-4-methoxy-phenyl)-[7-(4-trifluoromethyl-phenyl)-2,3-dihydro-pyrido[2,3-b][1,4]oxazin-1-yl]-methanone (122 mg, 0.21 mmol), lithium bromide (148 mg, 1.71 mmol) and piperazine (28 mg, 0.32 mmol) were dissolved in 3 ml of N,N-dimethyl formamide and then stirred at 1000 for 2 hours. After completion of the reaction by adding water dropwise, the mixture was adjusted to weak acidic condition (pH=6) by using 1N hydrochloric acid. The formed solid was filtered and washed with distilled water. The resulting solid was recrystallized from tetrahydrofuran and methanol to obtain the target compound 45, i.e., (3,5-dibromo-4-hydroxy-phenyl)-[7-(4-trifluoromethyl-phenyl)-2,3-dihydro-pyrido[2,3-b][1,4]oxazin-1-yl]-methanone (59 mg, 50%).

1. customAfter completion of the reaction
2. filtrationThe formed solid was filtered
3. washwashed with distilled water
4. customThe resulting solid was recrystallized from tetrahydrofuran and methanol

ORDレコード

ord-57d1b24c5b3a4b5f9f448668a854596f

出典データセット

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08394792B2