Hydrochloric Acid → HCID 54562540, compound

HRID 726880Notes

Reaction equation

HRID 726880 reaction equation
[OH-].[K+].[CH3:3][O:4][C:5]1[C:12]([O:13][CH3:14])=[CH:11][CH:10]=[CH:9][C:6]=1[CH:7]=O.[C:15]([OH:20])(=[O:19])[C:16]([CH3:18])=[O:17].Cl>C(Cl)Cl.CO.C(O)(=O)C.O.C(O)C>[O:17]=[C:16]([CH:18]=[CH:7][C:6]1[CH:9]=[CH:10][CH:11]=[C:12]([O:13][CH3:14])[C:5]=1[O:4][CH3:3])[C:15]([OH:20])=[O:19]

Participants

8

Reactant 4

HCID 313Hydrochloric AcidHCID 1060Pyruvic AcidHCID 14797Potassium HydroxideHCID 665812,3-Dimethoxybenzaldehyde

Product 1

HCID 54562540HCID 54562540, compound

Reagents, catalysts & solvents 3

HCID 702EthanolSolventHCID 962WaterSolvent2×HCID 21877243DCM MeOH AcOHSolvent

Procedure

300 ml of deionized water and 50 g of potassium hydroxide are placed into a 3 l flask. The mixture is stirred until dissolution, then 150 ml of ethanol and 100 g of 2,3-dimethoxybenzaldehyde are added. After that, 60.0 g of pyruvic acid are dropped therein (in about 30 minutes) and the mixture is stirred for about 15 minutes at a temperature from 35° to 40° C., then it is poured into 6500 ml of water and brought to markedly acid pH with about 140 ml of concentrated HCl. The mixture is cooled with stirring for about 30 minutes, then filtered washing with water and dried under Vacuum at 60° C. to obtain an orange solid. Yield: 115 g, 81% (moles), 115% (weight); TLC: methylene chloride/methanol/acetic acid 80/20/2; Rf=0,5; M.P.: 136°-138° C.

Workup

  1. stirring(in about 30 minutes) and the mixture is stirred for about 15 minutes at a temperature from 35° to 40° C.
  2. temperatureThe mixture is cooled
  3. stirringwith stirring for about 30 minutes
  4. filtrationfiltered
  5. washwashing with water
  6. customdried under Vacuum at 60° C.
  7. customto obtain an orange solid

Sources & evidence

ORD record
ord-b344c3f271e1471cbe34af69d3cf820f
Source dataset
uspto-grants-1998_01
Patent number
US05710336

Reaction notes

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