Methane → Cefdinir monohydrate

HRID 969252

反応式

HRID 969252 の反応式
[CH2:1]=[CH:2][C:3]1[CH2:23][S:22][C@@H:6]2[C@H:7]([NH:10][C:11](/[C:13](/[C:16]3[N:20]=[C:19]([NH2:21])[S:18][CH:17]=3)=[N:14]\[OH:15])=[O:12])[C:8](=[O:9])[N:5]2[C:4]=1[C:24]([OH:26])=[O:25].C(=O)(O)[O-:28].[Na+].C>O>[CH2:1]=[CH:2][C:3]1[CH2:23][S:22][C@@H:6]2[C@H:7]([NH:10][C:11](/[C:13](/[C:16]3[N:20]=[C:19]([NH2:21])[S:18][CH:17]=3)=[N:14]\[OH:15])=[O:12])[C:8](=[O:9])[N:5]2[C:4]=1[C:24]([OH:26])=[O:25].[OH2:28]

参加物

5

反応物 3

HCID 297MethaneHCID 516892Sodium BicarbonateHCID 6915944Cefdinir

生成物 1

HCID 11993766Cefdinir monohydrate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

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.

後処理

  1. washeluted with 20% aqueous acetone
  2. concentrationconcentrated to 200 ml
  3. customwas adjusted to pH 2.2 at 15° C. with 10% hydrochloric acid
  4. filtrationThe resultant crystals were collected by filtration
  5. washwashed with water
  6. customdried

出典と根拠

ORDレコード
ord-ad9dcb1ebd824545b2dd18942824fe49
出典データセット
uspto-grants-2007_12
特許番号
US07307072B2

関連ノート

読み込み中…