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Ethyl Acetate → 5-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2H-Isoindole-2-acetyl chloride, 1,3-dihydro-1,3-dioxo- | HCID 81242 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 5-chloro-2-(3-aminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone dihydrobromide | HCID 21325736 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone | HCID 15567871 | 69.4% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04147700 |
| 出典データセット | uspto-grants-1979_04 |
| ORD ID | ord-fa5c1e1f50024435931f8a587a320208 |
| 出典メモ | uspto-grants-1979_04 |