反应详情

The procedure of Example 1 was employed utilizing N-3-methylphenyl-N-benzylamine and phenyl phosphonic dichloride. The reaction of the dilithio compound and the phenyl phosphonic dichloride was conducted at 0° C. The crude product produced as a result of the chromatographic separation was crystallized from diethyl ether then recrystallized from carbon tetrachloride to yield 1-phenyl-2-(3-methylphenyl)-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide as a yellow solid. A second crop was obtained to give a total yield of 1.2 g (12% yield) of 1-phenyl-2-(3-methylphenyl)-2,3-dihydro-1H-2,1-benzazaphosphole-1-oxide having a melting point of 190°-192° C. and the following analysis:

1. customwas conducted at 0° C
2. customThe crude product produced as
3. customa result of the chromatographic separation
4. customwas crystallized from diethyl ether
5. customthen recrystallized from carbon tetrachloride