関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | 1,1-Difluoro-2-iodoethane | HCID 3833565 | — |
| 反応物 | HCID 67170227 | HCID 67170227 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(1-(2,2-Difluoroethyl)piperidin-4-ylamino)-3-nitrobenzenesulfonamide | HCID 48934007 | — |
反応手順
3-nitro-4-(piperidin-4-ylamino)benzenesulfonamide hydrochloride (0.100 g), 1,1-difluoro-2-iodoethane (0.063 mL) and diisopropylamine (0.156 mL) were stirred together in N,N-dimethylformamide (3 ml) and heated to 85° C. The reaction was diluted with dichloromethane (50 mL) and washed with water (50 mL), brine (50 mL), dried over magnesium sulfate, filtered, and concentrated. The residue was loaded onto silica gel (GraceResolve 12 g) and eluted using a gradient of 0.5% methanol/dichloromethane to 3% methanol/dichloromethane over 30 minutes to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08546399B2 |
|---|
| 出典データセット | uspto-grants-2013_10 |
|---|
| ORD ID | ord-2d0fe213544440559d835dc317332f00 |
|---|
| 出典メモ | uspto-grants-2013_10 |
|---|