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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
The procedure is analogous to that described in Example 1, but starting with benzoic acid (12.6 g), N,N'-carbonyldiimidazole (7.45 g) and 2-amino-7-(4-chlorophenoxy)-1,8-naphthyridine (12.6 g). The product obtained by precipitation in water (13 g; m.p. 100° C.) is purified by chromatography on a 4-cm-diameter column containing silica (0.040-0.063 mm; 200 g), eluting with methylene chloride and collecting 100-cc fractions. The fractions 10 to 25 are concentrated to 9/10 of the initial volume. After cooling for 2 hours at 0° C., the crystallized solid is separated by filtration, washed with diethyl ether (2×5 cc) and dried at 40° C. under reduced pressure (0.07 kPa). N-[7-(4-chlorophenoxy)-1,8-naphthyridin-2-yl]benzamide (4 g), m.p. 148° C., is obtained.
WORKUP
后处理
- customis purified by chromatography on a 4-cm-diameter column
- additioncontaining silica (0.040-0.063 mm; 200 g)
- washeluting with methylene chloride
- customcollecting 100-cc fractions
- concentrationThe fractions 10 to 25 are concentrated to 9/10 of the initial volume
- customthe crystallized solid is separated by filtration
- washwashed with diethyl ether (2×5 cc)
- customdried at 40° C. under reduced pressure (0.07 kPa)