تفاعل #1379889

ord-02e64fcc1c34429789c49e94ff5532f7

معادلة التفاعل

[Na+].[OH-]
sodium hydroxide
COC(=O)c1ccc(Nc2cccc3ncccc23)cc1
product
COC(=O)c1ccc(Nc2cccc3ncccc23)cc1
4-(quinolin-5-ylamino)-benzoic Acid Methyl Ester
O=C(O)c1ccc(Nc2cccc3ncccc23)cc1
orange powder
O=C(O)c1ccc(Nc2cccc3ncccc23)cc1
4-(quinolin-5-ylamino)-benzoic Acid

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىwas removed under reduced pressure
  2. 2
    أخرىThe resultant residue was purified
  3. 3
    workup.DISSOLUTIONby dissolving in water (1000 ml)
  4. 4
    أخرىprecipitating the crude product by acidification to pH3 with 2N HCl
  5. 5
    أخرىThe precipitate so formed
  6. 6
    ترشيحwas collected by filtration
  7. 7
    غسيلwashed with water (250 ml)
  8. 8
    أخرىThis purification procedure
  9. 9
    أخرىwas dried

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07238228B2uspto-grants-2007_07