関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (S)-1-(2-Fluorophenyl)ethylamine | HCID 7023579 | — |
| 反応物 | 5-(3-Bromophenyl)-2-methoxy-5,6,6-trimethyl-5,6-dihydro-1,4,3-oxathiazine 4,4-dioxide | HCID 68359171 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178462012 | HCID 178462012 | 62.8% |
反応手順
A solution of 209 mg of 5-(3-bromophenyl)-2-methoxy-5,6,6-trimethyl-5,6-dihydro-1,4,3-oxathiazine 4,4-dioxide and 92 mg of (S)-1-(2-fluorophenyl)ethylamine in 5 ml of methylene chloride was stirred at room temperature for 1 hour and the conversion was checked by LCMS. Since no conversion had taken place yet, the solvent was concentrated by rotary evaporation and the residue was stirred at room temperature for 19 hours. The crude product was purified by means of normal phase chromatography using a Flashmaster with an n-heptane/ethyl acetate gradient. The product-containing fractions were combined and concentrated by rotary evaporation. This gave the product (170 mg) with a molecular weight of 469.4 g/mol (C20H22BrFN2O3S); MS (ESI): m/e=469 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08895547B2 |
|---|
| 出典データセット | uspto-grants-2014_11 |
|---|
| ORD ID | ord-d90dd1d3fdd44c2e9bf407e0efe1df8a |
|---|
| 出典メモ | uspto-grants-2014_11 |
|---|