HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 5-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 2H-Isoindole-2-acetyl chloride, 1,3-dihydro-1,3-dioxo- | HCID 81242 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 5-chloro-2-(3-aminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone dihydrobromide | HCID 21325736 | — |
| Solvent | Benzene | HCID 241 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 5-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone | HCID 15567871 | 69.4% |
Reaction Steps
To a solution of 2-phthalimidoacetyl chloride (1.5 g) in benzene (20 ml) and dimethylformamide (10 ml), 5-chloro-2-(3-aminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone dihydrobromide (2.3 g) is added under ice cooling and stirring, and the temperature within the flask is gradually returned to room temperature. The reaction mixture is allowed to stand at room temperature, neutralized with saturated aqueous sodium bicarbonate, and shaken with ethyl acetate. The precipitated crystals are filtered, washed with methanol and dried to give 5-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone (1.68 g) as crystals melting at 251°-253° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04143048 |
| Source dataset | uspto-grants-1979_03 |
| ORD ID | ord-7b823883da4a4fdf95457f201a2c32df |
| Source note | uspto-grants-1979_03 |