HCID 86748173, compound → HCID 86748172, compound

HRID 1707324Notes

Reaction equation

HRID 1707324 reaction equation
[CH:1]1[CH:2]=[CH:3][C:4]([C@@H:7]([NH2:24])[C:8]([NH:10][C@@H:11]2[C:18](=[O:19])[N:17]3[C@@H:12]2[CH2:13][CH2:14][C:15]([Cl:23])=[C:16]3[C:20]([OH:22])=[O:21])=[O:9])=[CH:5][CH:6]=1.[CH3:25]N(C=O)C>CC(C)=O>[CH:1]1[CH:2]=[CH:3][C:4]([C@@H:7]([NH2:24])[C:8]([NH:10][C@@H:11]2[C:18](=[O:19])[N:17]3[C@@H:12]2[CH2:13][CH2:14][C:15]([Cl:23])=[C:16]3[C:20]([OH:22])=[O:21])=[O:9])=[CH:5][CH:6]=1.[CH3:25][C:20]([CH3:16])=[O:22]

Participants

3

Reactant 1

HCID 86748173HCID 86748173, compound

Product 1

HCID 86748172HCID 86748172, compoundYield 101.5%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

Loracarbef DMF disolvate 7.0 g (50 bg) was slurried in 50 ml acetone for 15 minutes (no noticeable change under microscope). The crystals were filtered on a 5.5 cm Buchner funnel with a Whatman 1 filter (fast filtration). The crystals were washed with ~7 ml acetone. The crystals were dried in the vacuum oven for two hours at 45° C. Wgt: 5.66 g, Purity: 90.4%, DMF: 3.15%, KF: 4.3%, Rel. Subs: 0.23%, Yield: 101.5%

Workup

  1. filtrationThe crystals were filtered on a 5.5 cm Buchner funnel with a Whatman 1
  2. filtrationfilter
  3. filtration(fast filtration)
  4. washThe crystals were washed with ~7 ml acetone
  5. customThe crystals were dried in the vacuum oven for two hours at 45° C

Sources & evidence

ORD record
ord-e7b1f7986730400ba6eea8ca1930288c
Source dataset
uspto-grants-1994_10
Patent number
US05352782

Reaction notes

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