Hydrochloric Acid → HCID 178489905, compound

HRID 1766057Notes

Reaction equation

HRID 1766057 reaction equation
S(O)(O)(=O)=O.[CH3:6][S:7][C:8](=[NH:10])[NH2:9].[CH3:11][O:12][C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[CH:16]=O.[C:21]([CH2:23][C:24](OCC)=[O:25])#[N:22].C(=O)([O-])[O-].[K+].[K+].Cl>C(O)C>[C:21]([C:23]1[C:16]([C:15]2[CH:18]=[CH:19][CH:20]=[C:13]([O:12][CH3:11])[CH:14]=2)=[N:10][C:8]([S:7][CH3:6])=[N:9][C:24]=1[OH:25])#[N:22]

Participants

7

Reactant 5

HCID 313Hydrochloric AcidHCID 7764Ethyl cyanoacetateHCID 11430Potassium CarbonateHCID 115693-MethoxybenzaldehydeHCID 752702-Methyl-2-thiopseudourea sulfate

Product 1

HCID 178489905HCID 178489905, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
0 °C

Procedure

A mixture of S-methylisothiourea sulfate (139 mg), 3-methoxybenzaldehyde (243 μl), ethyl cyanoacetate (112 μl) and potassium carbonate (145 mg) in abs. ethanol (2 ml) was stirred at 60° C. for 5 h. The reaction mixture was cooled to 0° C. in an ice bath, filtered and the residue was heated in water (H2O) until a clear solution was obtained. The solution was acidified with 2N aq. HCl to pH 2 and cooled to 0° C. in an ice bath. The resulting crystals were collected by filtration and dried in vacuo.

Workup

  1. filtrationfiltered
  2. temperaturethe residue was heated in water (H2O) until a clear solution
  3. customwas obtained
  4. temperaturecooled to 0° C. in an ice bath
  5. filtrationThe resulting crystals were collected by filtration
  6. customdried in vacuo

Sources & evidence

ORD record
ord-1b6563b6873c45168dcfde0140d5799d
Source dataset
uspto-grants-2007_06
Patent number
US07229990B2

Reaction notes

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