反应 #1379889

反应方程式

sodium hydroxide

product

4-(quinolin-5-ylamino)-benzoic Acid Methyl Ester

→

orange powder

4-(quinolin-5-ylamino)-benzoic Acid

溶剂

water

tetrahydrofuran

methanol

反应条件

后处理

1. 1
   其他was removed under reduced pressure
2. 2
   其他The resultant residue was purified
3. 3
   workup.DISSOLUTIONby dissolving in water (1000 ml)
4. 4
   其他precipitating the crude product by acidification to pH3 with 2N HCl
5. 5
   其他The precipitate so formed
6. 6
   过滤was collected by filtration
7. 7
   洗涤washed with water (250 ml)
8. 8
   其他This purification procedure
9. 9
   其他was dried

实验过程

A solution of sodium hydroxide (7 g, 0.18 mol) in water (100 ml) was added to a solution of the product from stage (a) in a mixture of tetrahydrofuran (100 ml) and methanol (350 ml). The reaction mixture was stirred at 50° C. for 3 h before the solvent was removed under reduced pressure. The resultant residue was purified by dissolving in water (1000 ml) adjusted to pH10 with 2M NaOH and precipitating the crude product by acidification to pH3 with 2N HCl. The precipitate so formed was collected by filtration and washed with water (250 ml). This purification procedure was repeated a further two times before the product was dried to give 12.3 g of an orange powder.

来源