Ammonia → Cephalexin Monohydrate

HRID 454793

Reaction equation

HRID 454793 reaction equation
[CH3:1][C:2]1[CH2:21][S:20][C@@H:5]2[C@H:6]([NH:9][C:10]([C@H:12]([NH2:19])[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)=[O:11])[C:7](=[O:8])[N:4]2[C:3]=1[C:22]([OH:24])=[O:23].N>O>[CH3:1][C:2]1[CH2:21][S:20][C@@H:5]2[C@H:6]([NH:9][C:10]([C@H:12]([NH2:19])[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)=[O:11])[C:7](=[O:8])[N:4]2[C:3]=1[C:22]([OH:24])=[O:23].[OH2:8]

Participants

4

Reactant 2

HCID 222AmmoniaHCID 27447Cephalexin2×

Product 1

HCID 62921Cephalexin MonohydrateYield 6,198.5%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
20 °C

Procedure

A crystallization reactor was filled with 20 g water and 1.0 g of cephalexin (seed). The above-mentioned acidic cephalexin solution was dosed into the crystallization reactor in 80 minutes at 30° C. The pH was kept at 5.0 with ammonia. Subsequently, the suspension was stirred at 20° C. for another 30 min. The suspension was filtered through a glass filter and the wet cake was washed with 2×15 ml water and 2×15 ml acetone. After drying, 32.6 g cephalexin monohydrate was obtained (purity ≧99.8%).

Workup

  1. filtrationThe suspension was filtered through a glass
  2. filtrationfilter
  3. washthe wet cake was washed with 2×15 ml water and 2×15 ml acetone
  4. customAfter drying

Sources & evidence

ORD record
ord-c7df748c2f4f4fda951ded7921fe5f1a
Source dataset
uspto-grants-2013_07
Patent number
US08497088B2

Linked notes

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