HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 91477957, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 57973784 | HCID 57973784 | — |
| Reactant | HCID 57973796 | HCID 57973796 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 91477957 | HCID 91477957 | — |
Reaction Steps
A mixture of 207 mg (0.6 mmol) of tert-butyl[(1R)-3-hydrazino-3-oxo-1-(2,4,5-trifluorobenzyl)propyl]carbamate (Intermediate 4), 110 mg (0.5 mmol) of 3-(trifluoromethyl)-6,7-dihydro[1,2,4]triazolo[4,3-a]pyrazine-8(5H)-thione (Intermediate 6), and 5.5 mL of methanol was stirred at reflux for 1 day. Diethyl ether was added to the cooled solution, resulting in precipitation. The solid was removed by filtration, and the filtrate was concentrated to dryness. Purification of the residue by preparative HPLC (C18 reverse phase column, 30-80% acetonitrile in water containing 0.05% trifluoroacetic acid) afforded the title compound. LC-MS 536 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07625888B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-7570d26c96434153b623cc6e9ec52412 |
| Source note | uspto-grants-2009_12 |