HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 178518183, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 117839340 | HCID 117839340 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178518183 | HCID 178518183 | 15% |
Reaction Steps
To (R)-4-chloro-N-[1-(4-fluorophenyl)pyrrolidin-3-yl]-1,3,5-triazin-2-amine synthesized in Reference Synthesis Example 337, sodium acetate (153 mg, 1.11 mmol), acetic acid (2.0 mL), and water (0.40 mL) were added and the resultant mixture was stirred at 90° C. for 5 hours. After completion of the reaction, the reaction solution was added to saturated sodium bicarbonate aqueous solution and extraction from the resultant mixture with ethyl acetate was performed. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure and the obtained solid was washed with ethyl acetate to obtain the title compound (65.0 mg, two step yield 15%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403798B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-10dbf37392df4646b31d5a0bfa87072b |
| Source note | uspto-grants-2016_08 |