関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,4-Dimethoxystyrene | HCID 61400 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| 反応物 | HCID 178480083 | HCID 178480083 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 178489978 | HCID 178489978 | 66% |
反応手順
A flask was charged with 5-(2,4-Bis-benzyloxy-5-bromo-phenyl)-4-(1-methyl-1H-indol-5-yl)-4H-[1,2,4]triazol-3-ol (290 mg; 0.50 mmol), 3,4-dimethoxystyrene (98 mg; 0.60 mmol), tris(dibenzylideneacetone)dipalladium(0) (11 mg; 0.025 eq.), tris-tert-butylphosphine (10 mg; 0.10 eq.), diisopropylethylamine (77 mg; 0.60 mmol), and dimethylformamide (2 mL). The reaction was heated at 135° C. overnight, and then cooled. The solution was diluted with ethyl acetate (40 mL) and washed with water (3×40 mL). The organic layer was dried with sodium sulfate, evaporated, and purified by column chromatography to give 5-{2,4-bis-benzyloxy-5-[2-(3,4-dimethoxy-phenyl)-vinyl]-phenyl}-4-(1-methyl-1H-indol-5-yl)-4H-[1,2,4]triazol-3-ol (220 mg; 0.33 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08927548B2 |
|---|
| 出典データセット | uspto-grants-2015_01 |
|---|
| ORD ID | ord-3c590ee811f548ed9f1440c4c85bec48 |
|---|
| 出典メモ | uspto-grants-2015_01 |
|---|
