関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic anhydride | HCID 9845 | — |
| 反応物 | 2-(2,4-difluorophenyl)-4,5-dimethyl-2H-1,2,3-triazole 1-oxide | HCID 90109810 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(2,4-Difluorophenyl)-5-methyl-2H-1,2,3-triazole-4-methanol | HCID 90109252 | — |
反応手順
To a solution of 2-(2,4-difluorophenyl)-4,5-dimethyl-2H-1,2,3-triazole 1-oxide (i.e. the product of Step A, 1.78 g, 7.0 mmol) in tetrahydrofuran (14 mL) was added trifluoroacetic anhydride (2.5 mL, 17.5 mmol). The reaction mixture was stirred at 110° C. in the microwave for 75 min. The mixture was diluted with ethyl acetate, washed successively with 1.0 M aqueous sodium hydroxide and 50% aqueous sodium hydroxide, dried (MgSO4) and concentrated under reduced pressure to afford the crude product. The crude material was purified by chromatography on silica gel eluting with 0 to 100% ethyl acetate in hexanes to obtain the title compound (0.59 g) as a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09302999B2 |
|---|
| 出典データセット | uspto-grants-2016_04 |
|---|
| ORD ID | ord-9ac76b9069f9454cbc7121c5c424d5ac |
|---|
| 出典メモ | uspto-grants-2016_04 |
|---|