تفاعل #985265

ord-52f6304a211841e38c522993a859a60c

معادلة التفاعل

C
charcoal
C=CC1=C(C(=O)O)N2C(=O)[C@@H](NC(=O)/C(=N\O)c3csc(N)n3)[C@H]2SC1
Cefdinir
O=C([O-])O.[Na+]
sodium bicarbonate
C=CC1=C(C(=O)O)N2C(=O)[C@@H](NC(=O)/C(=N\O)c3csc(N)n3)[C@H]2SC1.O
Cefdinir monohydrate

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلeluted with 20% aqueous acetone
  2. 2
    تركيزconcentrated to 200 ml
  3. 3
    أخرىwas adjusted to pH 2.2 at 15° C. with 10% hydrochloric acid
  4. 4
    ترشيحThe resultant crystals were collected by filtration
  5. 5
    غسيلwashed with water
  6. 6
    أخرىdried

الإجراء التجريبي

The monohydrate was prepared as follows: Cefdinir (20.0 g) was added to water (200 ml) and the mixture was adjusted to pH 6.0 with saturated sodium bicarbonate aqueous solution. The resultant solution was subjected to a column chromatography on activated charcoal and eluted with 20% aqueous acetone. Fractions were combined and then concentrated to 200 ml. This solution was adjusted to pH 2.2 at 15° C. with 10% hydrochloric acid and stirred at 0° C. for 30 minutes. The resultant crystals were collected by filtration, washed with water and dried to give crystals of Cefdinir monohydrate. The present inventors investigated physicochemical properties for Cefdinir monohydrate and crystal form A. The results are described below.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07351419B2uspto-grants-2008_04