반응 #1379889

반응 방정식

sodium hydroxide

product

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

→

orange powder

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

용매

water

tetrahydrofuran

methanol

반응 조건

후처리

1. 1
   기타was removed under reduced pressure
2. 2
   기타The resultant residue was purified
3. 3
   workup.DISSOLUTIONby dissolving in water (1000 ml)
4. 4
   기타precipitating the crude product by acidification to pH3 with 2N HCl
5. 5
   기타The precipitate so formed
6. 6
   여과was collected by filtration
7. 7
   세척washed with water (250 ml)
8. 8
   기타This purification procedure
9. 9
   기타was dried

실험 절차

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.

출처