HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 58289917, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | HCID 58289879 | HCID 58289879 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 58289917 | HCID 58289917 | — |
Reaction Steps
211 μL of 1,8-diazabicyclo[5,4,0]undec-7-ene and 105 μL of methyl iodide were added to an N,N-dimethylformamide (5 mL) solution of 500 mg of 3-(2,6-dichlorophenyl)-7-(methylthio)pyrimido[4,5-d]pyrimidin-2,4(1H,3H)-dione obtained in Production Example 52, and stirred at room temperature for 1 hour. The reaction solution was added to ethyl acetate and aqueous 0.5 N hydrochloric acid solution with stirring, 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 crude product was solidified with methanol to obtain 420 mg of the entitled compound as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08436004B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-edb957f0a76842d4b3ed9a7d26694c77 |
| Source note | uspto-grants-2013_05 |