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Methane → Cefadroxil Monohydrate

HRID 224936
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HRID 224936 반응식
[CH3:1][C:2]1[CH2:22][S:21][C@@H:5]2[C@H:6]([NH:9][C:10]([C@H:12]([NH2:20])[C:13]3[CH:14]=[CH:15][C:16]([OH:19])=[CH:17][CH:18]=3)=[O:11])[C:7](=[O:8])[N:4]2[C:3]=1[C:23]([OH:25])=[O:24].CN(C=[O:30])C.Cl.C>O>[CH3:1][C:2]1[CH2:22][S:21][C@@H:5]2[C@H:6]([NH:9][C:10]([C@H:12]([NH2:20])[C:13]3[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=3)=[O:11])[C:7](=[O:8])[N:4]2[C:3]=1[C:23]([OH:25])=[O:24].[OH2:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 297MethaneHCID 313Hydrochloric AcidHCID 86754917HCID 86754917, 화합물

생성물 1

HCID 47964Cefadroxil Monohydrate수율 76%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Cefadroxil DMF solvate (50 g.; ~0.105 mole) was dissolved in 150 ml. water and 8.8 ml. HCl (36%). Charcoal (2.7 g.) and Celite (1.35 g.) were then added. After 30 minutes of stirring, the mixture was filtered through a Celite pad and washed with water. The filtered solution was heated to 40° and the pH adjusted to 2.5 with triethylamine. The mixture was then seeded with crystals of cefadroxil monohydrate and the pH adjusted to 4.5 with triethylamine. The suspension was stirred for one hour at 50° and progressively cooled to room temperature and then maintained for one hour at 0° to +5°. The crystalline cefadroxil monohydrate was collected, washed twice with cold water and dried at 40° to yield 30.8 g. (~76-77% yield) of product having the same physical characteristics as described in Example 1.

후처리

  1. filtrationthe mixture was filtered through a Celite pad
  2. washwashed with water
  3. temperatureThe filtered solution was heated to 40°
  4. stirringThe suspension was stirred for one hour at 50°
  5. temperaturemaintained for one hour at 0° to +5°
  6. customThe crystalline cefadroxil monohydrate was collected
  7. washwashed twice with cold water
  8. customdried at 40°
  9. customto yield 30.8 g

출처 및 근거

ORD 기록
ord-2a3a8b3773ab486ba601ca5b0a14aa89
출처 데이터셋
uspto-grants-1980_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04234721

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