Oxalic Acid → HCID 86623396, compound

HRID 549971Notes

Reaction equation

HRID 549971 reaction equation
[CH3:1][N:2]([CH2:4][CH2:5][C:6]1[C:10]2[CH:11]=[C:12]([CH2:15][S:16]([N:19]3[CH2:23][CH2:22][CH2:21][CH2:20]3)(=[O:18])=[O:17])[CH:13]=[CH:14][C:9]=2[NH:8][CH:7]=1)[CH3:3].[C:24]([OH:29])(=[O:28])[C:25]([OH:27])=[O:26]>C(O)C>[CH3:1][N:2]([CH2:4][CH2:5][C:6]1[C:10]2[CH:11]=[C:12]([CH2:15][S:16]([N:19]3[CH2:23][CH2:22][CH2:21][CH2:20]3)(=[O:18])=[O:17])[CH:13]=[CH:14][C:9]=2[NH:8][CH:7]=1)[CH3:3].[C:24]([O-:29])(=[O:28])[C:25]([O-:27])=[O:26]

Participants

4

Reactant 2

HCID 971Oxalic AcidHCID 123606Almotriptan

Product 1

HCID 86623396HCID 86623396, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
0 °C

Procedure

Almotriptan crude (10 gms, purity 92.5%) is dissolved in Ethanol (60 ml) at room temperature. Reaction mass is stirred for 15 min for the complete dissolution. Oxalic Acid solution (4.0 gms in 15 ml Ethanol) is added to the above solution over 30 min at room temperature. Reaction mass temperature is raised to reflux and maintained for about 6 hrs. Slowly cooled the reaction mass to 0° C. and maintained for about 1 hr at 0±3° C. The precipitated material is filtered and washed with 15 ml of Ethanol.

Workup

  1. customReaction mass
  2. customReaction mass temperature
  3. temperatureis raised
  4. temperatureto reflux
  5. temperaturemaintained for about 6 hrs
  6. temperaturemaintained for about 1 hr at 0±3° C
  7. filtrationThe precipitated material is filtered
  8. washwashed with 15 ml of Ethanol

Sources & evidence

ORD record
ord-790a869fa4d748d5880731647cf0fa77
Source dataset
uspto-grants-2011_05
Patent number
US07943784B2

Reaction notes

Loading…