反応 #985265

ord-52f6304a211841e38c522993a859a60c

反応方程式

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

溶媒

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄eluted with 20% aqueous acetone
  2. 2
    濃縮concentrated to 200 ml
  3. 3
    その他was adjusted to pH 2.2 at 15° C. with 10% hydrochloric acid
  4. 4
    ろ過The resultant crystals were collected by filtration
  5. 5
    洗浄washed with water
  6. 6
    その他dried

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07351419B2uspto-grants-2008_04