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Sodium hydride → 5-n-Butyl-2,4-dihydro-2-[1-(carbomethoxy)ethyl]-4-[(2'-cyanobiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methyl 2-bromopropionate | HCID 95576 | — |
| 反応物 | 4'-[(3-butyl-5-oxo-1,5-dihydro-4H-1,2,4-triazol-4-yl)methyl]biphenyl-2-carbonitrile | HCID 14951052 | — |
| 生成物 | 5-n-Butyl-2,4-dihydro-2-[1-(carbomethoxy)ethyl]-4-[(2'-cyanobiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one | HCID 14956822 | 84% |
反応手順
The alkylation of 5-n-butyl-4-[(2'-cyanobiphenyl-4-yl)methyl)-2,4-dihydro-3H-1,2,4-triazol-3-one (from Example 9, Step C) with methyl 2-bromopropionate was carried out as described in Example 3, Step A, except that no excess sodium hydride was used. After work-up, the residue was flash chromatographed over silica gel (eluted with 0.5% MeOH/CH2Cl2) to give the desired material in 84% yield as a colorless oil, homogeneous by TLC in 2% MeOH/CH2Cl2, mass spectrum (FAB) 419 (M+1)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05411980 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-d15377aa467143e7984753cb26e63cb6 |
| 出典メモ | uspto-grants-1995_05 |