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Sodium hydride → 5-n-Butyl-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]biphenyl-4-yl]methyl]-2-[2-chloro-5-(valerylamino)phenyl]-2,4-dihydro-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 | Valeryl chloride | HCID 61186 | — |
| 反応物 | 4''-[1-(5-Amino-2-chloro-phenyl)-3-butyl-5-oxo-1,5-dihydro-[1,2,4]triazol-4-ylmethyl]-biphenyl-2-sulfonic acid 2-chloro-benzoylamide | HCID 10032193 | — |
| 生成物 | 5-n-Butyl-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]biphenyl-4-yl]methyl]-2-[2-chloro-5-(valerylamino)phenyl]-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 10078663 | — |
反応手順
The title compound was prepared from 2-(5-amino-2-chlorophenyl)-5-n-butyl-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]biphenyl-4-yl]methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one (from Example 60), sodium hydride, and valeryl chloride according the procedure of Example 57. The crude product was flash chromatographed over silica gel (gradient elution with 0.5-2.0% MeOH/CH2Cl2) to give the desired compound as a cream-colored solid in 48% yield, mp >110° C. (gradual), homogeneous by TLC (9:1 MeOH/CH2Cl2), mass spectrum (FAB) m/e 734 (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-e3472501156347b7b2f8f4a608c55708 |
| 出典メモ | uspto-grants-1995_05 |