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Ethyl Acetate → 2-[5-Amino-2-(trifluoromethyl)phenyl]-5-n-butyl-4-[[2'-(N-t-butylsulfamoyl)biphenyl-4-yl]methyl]-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 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 5-n-Butyl-4-[[2'-(N-t-butylsulfamoyl)biphenyl-4-yl]methyl]-2,4-dihydro-2-[5-nitro-2-(trifluoromethyl)phenyl]-3H-1,2,4-triazol-3-one | HCID 10394261 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Platinum oxide (PtO) | HCID 82844 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-[5-Amino-2-(trifluoromethyl)phenyl]-5-n-butyl-4-[[2'-(N-t-butylsulfamoyl)biphenyl-4-yl]methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 10100136 | 100% |
反応手順
A mixture of 200 mg (0.317 mmole) of 5-n-butyl-4-[[2'-(N-t-butylsulfamoyl)biphenyl-4-yl]methyl]-2,4-dihydro-2-[5-nitro-2-(trifluoromethyl)phenyl] -3H-1,2,4-triazol-3-one (from Step C), 15 mg of platinum oxide, 10 mL of ethyl acetate, and 2 mL of ethanol was shaken with hydrogen at approximately 4 atm for a few hours until complete and then centrifuged. The supernatant was decanted off, and the catalyst pellet was extracted 3× with ethanol in the same manner. The combined supernatant fractions were concentrated to give 190 mg (100%) of the title compound as a brown foam, which was suitable for use without further purification; TLC in 95:5 CH2Cl2 --MeOH; mass spectrum (FAB) m/e 608 (M+Li)+.
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-29d18f6de15b47bbafe9026de493b6fe |
| 出典メモ | uspto-grants-1995_05 |