Sodium Carbonate → HCID 178503549, compound

HRID 2353640Notes

Reaction equation

HRID 2353640 reaction equation
S(O)(O)(=O)=O.[CH3:6][S:7][C:8](=[NH:10])[NH2:9].[Cl:11][CH2:12][C:13](=O)[CH2:14][C:15](OCC)=[O:16].C(=O)([O-])[O-].[Na+].[Na+]>O>[Cl:11][CH2:12][C:13]1[N:9]=[C:8]([S:7][CH3:6])[N:10]=[C:15]([OH:16])[CH:14]=1

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 69484Ethyl 4-chloroacetoacetateHCID 752702-Methyl-2-thiopseudourea sulfate

Product 1

HCID 178503549HCID 178503549, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

S-Methyl-2-thiopseudourea sulphate (20 g, 71.85 mmol), ethyl 4-chloroacetoacetate (10.755 ml, 79.04 mmol) and sodium carbonate (13.925 g, 107.78 mmol) were dissolved in water (100 ml) and stirred at room temperature overnight. The reaction was monitored by TLC, and once complete, the reaction precipitate was collected and the supernatant was neutralised with 6N hydrochloric acid to yield more reaction precipitate which was also collected. The accumulated precipitate was then washed with water (×3) and an off-white solid was obtained. This was dried in vacuo at 60° C. for 48 hours to yield the desired compound as a pale yellow/white solid, 43.2 g.

Workup

  1. customonce complete, the reaction precipitate was collected
  2. customto yield more
  3. customreaction precipitate which
  4. customwas also collected
  5. washThe accumulated precipitate was then washed with water (×3)
  6. customan off-white solid was obtained
  7. customThis was dried in vacuo at 60° C. for 48 hours

Sources & evidence

ORD record
ord-2115342f0cbd4b5a95e8a6005d9214d3
Source dataset
uspto-grants-2010_07
Patent number
US07750003B2

Reaction notes

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