HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 4-(4-Bromo-2-fluorobenzyl)-5-n-butyl-2-[5-(N-n-butylcarbamoyl)-2-chloro-phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 4-(4-Bromo-2-fluorobenzyl)-5-n-butyl-2-[2-chloro-5-(methoxycarbonyl)phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 10006049 | — |
| Solvent | Butylamine | HCID 8007 | — |
| Product | 4-(4-Bromo-2-fluorobenzyl)-5-n-butyl-2-[5-(N-n-butylcarbamoyl)-2-chloro-phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 10075899 | — |
Reaction Steps
A solution of 50 mg (0.10 mmol) of 4-(4-bromo-2-fluorobenzyl)-5-n-butyl-2-[2-chloro-5-(methoxycarbonyl)phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one (from Step D) in 1 mL of n-butylamine was stirred overnight at 65° C. and then evaporated in vacuo. The residue was flash chromatographed on 15 cc of silica gel (gradient elution with 1-5% MeOH in CH2Cl2) to yield 41 mg (76%) of colorless, glassy solid, mp 114°-116° C.; homogeneous by TLC (95:5 CH2Cl2 --MeOH); mass spectrum (FAB) M/e 537, 539 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05281614 |
| Source dataset | uspto-grants-1994_01 |
| ORD ID | ord-cd16822b6198433b96877b285a738a2b |
| Source note | uspto-grants-1994_01 |