反应详情

In the apparatus described in Example 1, 25.4 g of 4-trichloromethylbenzoic acid methyl ester (0.1 mol) and 10.9 g of 2-aminophenol (0.1 mol) were mixed and slowly heated up to 200° C, so that the stream of HCl that commences at 130° C would not become too strong. The total reaction time was about 4 hours. The ground reaction product was washed thrice with 100 ml of hot benzene and the combined and concentrated benzene phases where chromatographed through an Al2O3 : 8.9 g of raw product XVI, melting point 190°-191° C (35% of the theory), becoming 193°-194° C after recrystallization from benzene.

1. additionwere mixed
2. customThe ground reaction product
3. washwas washed thrice with 100 ml of hot benzene
4. customthe combined and concentrated benzene phases where chromatographed through an Al2O3
5. custombecoming 193°-194° C
6. customafter recrystallization from benzene