HRID2413929

反应详情

EQUATION

反应方程式

HRID 2413929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customis purified by chromatography on a 4-cm-diameter column
  2. additioncontaining silica (0.040-0.063 mm; 200 g)
  3. washeluting with methylene chloride
  4. customcollecting 100-cc fractions
  5. concentrationThe fractions 10 to 25 are concentrated to 9/10 of the initial volume
  6. customthe crystallized solid is separated by filtration
  7. washwashed with diethyl ether (2×5 cc)
  8. customdried at 40° C. under reduced pressure (0.07 kPa)