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Propionyl bromide → N-[2-[4-[[3-butyl-5-oxo-1-[5-(propanoylamino)-2-(trifluoromethyl)phenyl]-1,2,4-triazol-4-yl]methyl]-3-fluorophenyl]phenyl]sulfonyl-2-chlorobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Propionyl bromide | HCID 69018 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | 2-[5-amino-2-(trifluoromethyl)phenyl]-5-n-butyl-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]-3-fluorobiphenyl-4-yl]methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 19939446 | — |
| 溶媒 | Dichloromethane methanol | HCID 21226129 | — |
| 生成物 | N-[2-[4-[[3-butyl-5-oxo-1-[5-(propanoylamino)-2-(trifluoromethyl)phenyl]-1,2,4-triazol-4-yl]methyl]-3-fluorophenyl]phenyl]sulfonyl-2-chlorobenzamide | HCID 10395335 | 60% |
反応手順
The title compound was synthesized by reaction of 2-[5-amino-2-(trifluoromethyl)phenyl]-5-n-butyl-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]-3-fluorobiphenyl-4-yl]methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one (from Step G) with propionyl bromide (3 equivalents) and DBU (1.1 equiv) according to the method of Example 69. The material was obtained in 60% yield as a pale yellow solid, mp 181°-183° C.; homogeneous by TLC in 9:1 CH2Cl2 -MeOH; mass spectrum (FAB) m/e 796 (M+K)+.
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-28b94c3178b9471c9dca3e858d554c9e |
| 出典メモ | uspto-grants-1995_05 |