Реакция #1379889

Уравнение реакции

sodium hydroxide

product

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

→

orange powder

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

Растворители

water

tetrahydrofuran

methanol

Условия реакции

Обработка

1. 1
   Другоеwas removed under reduced pressure
2. 2
   ДругоеThe resultant residue was purified
3. 3
   workup.DISSOLUTIONby dissolving in water (1000 ml)
4. 4
   Другоеprecipitating the crude product by acidification to pH3 with 2N HCl
5. 5
   ДругоеThe precipitate so formed
6. 6
   Фильтрацияwas collected by filtration
7. 7
   Промывкаwashed with water (250 ml)
8. 8
   ДругоеThis purification procedure
9. 9
   Другоеwas dried

Методика

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.

Источник