反応 #1379889

反応方程式

sodium hydroxide

product

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

→

orange powder

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

溶媒

water

tetrahydrofuran

methanol

反応条件

後処理

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

実験手順

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.

出典