Methane → Cefdinir monohydrate

HRID 898083

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HRID 898083 반응식
[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]

참가 물질

5

반응물 3

HCID 297MethaneHCID 516892Sodium BicarbonateHCID 6915944Cefdinir

생성물 1

HCID 11993766Cefdinir monohydrate

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-52f6304a211841e38c522993a859a60c
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07351419B2

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