Acetic Acid → HCID 86658840, compound

HRID 451342Notes

Reaction equation

HRID 451342 reaction equation
[C:1]([OH:4])(=[O:3])[CH3:2].[CH:5]1[C:10]2=[N:11][S:12][N:13]=[C:9]2[C:8]([NH:14][C:15]2[NH:19][CH2:18][CH2:17][N:16]=2)=[C:7]([Cl:20])[CH:6]=1>CC(C)=O>[CH:5]1[C:10]2=[N:11][S:12][N:13]=[C:9]2[C:8]([NH:14][C:15]2[NH:19][CH2:18][CH2:17][N:16]=2)=[C:7]([Cl:20])[CH:6]=1.[C:1]([O-:4])(=[O:3])[CH3:2]

Participants

4

Reactant 2

HCID 176Acetic AcidHCID 5487Tizanidine

Product 1

HCID 86658840HCID 86658840, compoundYield 95.5%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Conditions

Temperature
2.5 °C

Procedure

To 60 ml of acetic acid 40 g of the tizanidine base (99.15% HPLC) are gradually added under stirring and heating until a yellow solution is obtained at 70 to 80° C., to which 200 ml of acetone are added. Shortly thereafter crystallization begins. After cooling to 0 to 5° C. and aspiration 47.25 g of tizanidine acetate (i.e. 95.5% th.) are obtained.

Workup

  1. temperatureheating until a yellow solution
  2. additionare added
  3. customShortly thereafter crystallization

Sources & evidence

ORD record
ord-081713a973094570b691ce1d08562fff
Source dataset
uspto-grants-2013_07
Patent number
US08487113B2

Reaction notes

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