3-Mercaptopropionic Acid → 82697-77-6

HRID 647067Notes

Reaction equation

HRID 647067 reaction equation
CO[C:3]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][C:4]=1[CH:5]=O.[SH:13][CH2:14][CH2:15][C:16]([OH:18])=O.[C:19](=[O:22])([O-])[O-].[NH4+:23].[NH4+]>C1C=CC=CC=1>[CH3:12][O:11][C:9]1[CH:10]=[CH:3][C:4]([CH:5]2[S:13][CH2:14][CH2:15][C:16](=[O:18])[NH:23]2)=[CH:7][C:8]=1[O:22][CH3:19]

Participants

5

Reactant 3

HCID 65143-Mercaptopropionic AcidHCID 691752,4-DimethoxybenzaldehydeHCID 517111Ammonium Carbonate

Product 1

HCID 306803682697-77-6Yield 87%

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

A mixture of 16.6 g of 2,4-dimethoxybenzaldehyde, 10.6 g of 3-mercaptopropionic acid and 6 g of ammonium carbonate in 250 ml of benzene was refluxed for 3 hours in a reaction vessel provided with a Dean-Stark apparatus at 80° C. while removing the distilled water. The crystals which separated out after cooling the reaction mixture were collected by filtration and recrystallized from hot benzene to obtain the object, colourless minute acicular crystals melting at 166° to 167° C. in an amount of 22 g corresponding to a yield of 87%.

Workup

  1. temperaturewas refluxed for 3 hours in a reaction vessel
  2. customprovided with a Dean-Stark apparatus at 80° C.
  3. customwhile removing the distilled water
  4. customThe crystals which separated out
  5. temperatureafter cooling the reaction mixture
  6. filtrationwere collected by filtration
  7. customrecrystallized from hot benzene

Sources & evidence

ORD record
ord-812c56e1bc974b4aaa5199d9437e6691
Source dataset
uspto-grants-1983_10
Patent number
US04407799

Reaction notes

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