HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 178517893, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 6-Chloro-4-[4-(4-fluorophenyl)piperazin-1-yl]-1,3,5-triazin-2(1H)-one | HCID 136933047 | — |
| Catalyst | Palladium hydroxide | HCID 9942167 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178517893 | HCID 178517893 | 99% |
Reaction Steps
An acetic acid (15 mL)-water (35 mL) mixed solution of 6-chloro-4-[4-(4-fluorophenyl)piperazin-1-yl]-1,3,5-triazin-2(1H)-one (1.00 g, 3.23 mmol) synthesized in Reference Synthesis Example 2 and palladium hydroxide-activated carbon catalyst (100 mg) was stirred under hydrogen atmosphere at room temperature for 3 days. After completion of the reaction, the reaction solution was filtered with Celite and the filtered residue was washed with methanol, followed by concentrating the obtained solution under reduced pressure. Toluene was added to the residue and the mixture was azeotropically dehydrated four times. The obtained residue was dried under reduced pressure to obtain the title compound (876 mg, yield 99%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403798B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-0c38336ab92949b691340a14b220604c |
| Source note | uspto-grants-2016_08 |