関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Fluoro-2-nitrobenzotrifluoride | HCID 223094 | — |
| 反応物 | (S)-2-Methylpyrrolidine 4-methylbenzenesulfonate | HCID 44118660 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (S)-2-methyl-1-(4-nitro-3-(trifluoromethyl)phenyl)pyrrolidine | HCID 59395009 | 100.1% |
反応手順
To a solution of (S)-2-methylpyrrolidine tosylate (10.6 g, 41.2 mmol) in acetonitrile (85 mL) was added 4-fluoro-1-nitro-2-(trifluoromethyl)benzene (6.6 g, 31.7 mmol) dropwise and followed by triethylamine (11.0 mL, 79.3 mmol) dropwise. The reaction was heated at 82° C. for 16 h. The reaction was quenched with water and extracted with ethyl acetate. The organic layer was washed with 1N HCl, then dried over Na2SO4 and concentrated in vacuo to yield (S)-2-methyl-1-(4-nitro-3-(trifluoromethyl)phenyl)pyrrolidine (8.7 g, quantitative yield). LC/MS m/z 275.3 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08367660B2 |
|---|
| 出典データセット | uspto-grants-2013_02 |
|---|
| ORD ID | ord-5026c783114c4fe5bc0d8d53c1c77604 |
|---|
| 出典メモ | uspto-grants-2013_02 |
|---|
