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1,1'-Carbonyldiimidazole → 5-n-Butyl-2-[2-chloro-5-nitrophenyl]-2,4-dihydro-4-[[2'-[N-(2-phenoxybenzoyl)sulfamoyl]biphenyl-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 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | 2-Phenoxybenzoic acid | HCID 75237 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | 5-n-Butyl-2-(2-chloro-5-nitrophenyl)-2,4-dihydro-4-[(2'-sulfamoylbiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one | HCID 10325049 | — |
| 生成物 | 5-n-Butyl-2-[2-chloro-5-nitrophenyl]-2,4-dihydro-4-[[2'-[N-(2-phenoxybenzoyl)sulfamoyl]biphenyl-4-yl]methyl]-3H-1,2,4-triazol-3-one | HCID 19939396 | — |
反応手順
The title compound was prepared from 5-n-butyl-2-(2-chloro-5-nitrophenyl)-2,4-dihydro-4-[(2'-sulfamoylbiphenyl-4-yl)methyl]-3H-1,2,4-triazol-3-one (from Example 59, Step C) and 2-phenoxybenzoic acid (2.5 equivalents), CDI (2.5 equiv), and DBU (2.5 equiv) according to the procedure of Example 51. Flash chromatography of the crude product on silica gel (gradient elution with 0.5-1% MeOH in CH2Cl2) gave a 55% yield of the desired material as a stiff foam, homogeneous by TLC in 95:5 CH2Cl2 --MeOH; mass spectrum (FAB) m/e 738 (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-6b529437a9e046b2bb5236318f1eaae4 |
| 出典メモ | uspto-grants-1995_05 |