HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 58289879, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 5-Pyrimidinecarboxylic acid, 4-amino-2-(methylthio)-, ethyl ester | HCID 222666 | — |
| Reactant | 1,3-Dichloro-2-isocyanatobenzene | HCID 604537 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 58289879 | HCID 58289879 | 85.9% |
Reaction Steps
315 mg of sodium hydride was added to an N,N-dimethylformamide (15 mL) solution of 1.0 g of ethyl 4-amino-2-(methylthio)pyrimidin-5-carboxylate, and stirred at room temperature for 5 minutes. 970 mg of 2,6-dichlorophenylisocyanate was added to the reaction liquid, and stirred at room temperature for 1 hour. Ethyl acetate and aqueous 1 N hydrochloric acid solution were added to the reaction solution, and the organic layer was separated. This was washed with saturated saline water, dried with anhydrous sodium sulfate, and the solvent was evaporated away. The precipitated solid was solidified with methanol, and the solid was taken out through filtration to obtain 1.43 g of the entitled compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08436004B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-3084eec47ae74bd9a1ce600351f50920 |
| Source note | uspto-grants-2013_05 |