Hydrochloric Acid → HCID 23620956, compound

HRID 1735486Notes

Reaction equation

HRID 1735486 reaction equation
[NH2:1][CH:2]1[C:23](=[O:24])[N:4]2[C:5]([C:10]([O:12]CC3C=CC([N+]([O-])=O)=CC=3)=[O:11])=[C:6]([Cl:9])[CH2:7][S:8][C@H:3]12.[Sn].Cl>CO.O>[NH2:1][CH:2]1[C:23](=[O:24])[N:4]2[C:5]([C:10]([OH:12])=[O:11])=[C:6]([Cl:9])[CH2:7][S:8][C@H:3]12

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 5352426Tin atomHCID 676435564-Nitrobenzyl 7-amino-3-chloro-3-cephem-4-carboxylate

Product 1

HCID 23620956HCID 23620956, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolvent2×HCID 962WaterSolvent2×

Procedure

p-Nitrobenzyl 7-amino-3-chloro-3-cephem-4-carboxylate (10 gm) was suspended in a mixture of methanol (120 ml) and water (25 ml). Tin powder was charged at 30° C., followed by the addition of concentrated HCl (25 ml) in a methanol (20 ml) and water (5 ml) mixture over a period of 15 minutes. The reaction mixture was stirred for 1 hour. After completion of the reaction, aq. KHCO3 was added to bring the pH to 8.0, followed by the addition of activated carbon. After stirring for 10 minutes, the mixture was filtered. To the filtrate was added aq. HCl to bring the pH to 4.0. The product thus separated was filtered and dried. Yield: 3.9 g (68%).

Workup

  1. additionwas added
  2. additionfollowed by the addition of activated carbon
  3. stirringAfter stirring for 10 minutes
  4. filtrationthe mixture was filtered
  5. additionTo the filtrate was added aq. HCl
  6. customThe product thus separated
  7. filtrationwas filtered
  8. customdried

Sources & evidence

ORD record
ord-6048f6a62d2748b783df2937bc7d4c5f
Source dataset
uspto-grants-1996_07
Patent number
US05536830

Reaction notes

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