반응 #305477

ord-9685bcf8e3a64a488c436c1c11c66f45

반응 방정식

NC(=O)c1cc[n+](CC2=C(C(=O)O)N3C(=O)[C@@H](NC(=O)C(c4ccccc4)S(=O)(=O)O)[C@H]3SC2)cc1
Cefsulodin
CC(=O)[O-].[Na+]
sodium acetate
→
NC(=O)c1cc[n+](CC2=C(C(=O)[O-])N3C(=O)[C@@H](NC(=O)C(c4ccccc4)S(=O)(=O)[O-])[C@H]3SC2)cc1.[Na+]
cefsulodin sodium

반응물

NC(=O)c1cc[n+](CC2=C(C(=O)O)N3C(=O)[C@@H](NC(=O)C(c4ccccc4)S(=O)(=O)O)[C@H]3SC2)cc1
Cefsulodin
CC(=O)[O-].[Na+]
sodium acetate

시약

없음

용매

CN(C)C=O
DMF
O
water

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled in an ice bath
  2. 2
    workup.STIRRINGThe mixture was stirred at ice temperature for 10 more minutes
  3. 3
    기타was then placed in a refrigerator overnight
  4. 4
    여과The crystallized cefsulodin sodium was filtered
  5. 5
    기타dried
  6. 6
    온도using heat under reduced pressure to a water content of about 3.18% by weight

실험 절차

Cefsulodin (5.0762 g) was dissolved in 10 mL of DMF and cooled in an ice bath. To this cold, yellow, syrupy solution was added 1.1 eq. of sodium acetate in 15 mL of water with stirring. The mixture was stirred at ice temperature for 10 more minutes. The mixture was then placed in a refrigerator overnight. The crystallized cefsulodin sodium was filtered, dried using heat under reduced pressure to a water content of about 3.18% by weight. 2.82 g of cefsulodin sodium were obtained (63%). Microscopic analysis of the resulting crystals showed that the cefsulodin sodium was spherical-type crystals.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08198434B2uspto-grants-2012_06