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Dimethylformamide → 4-((1-(1,3-Difluoropropan-2-yl)-4-fluoropiperidin-4-yl)methoxy)-3-nitrobenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 1,3-Difluoroacetone | HCID 228397 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | 4((4-Fluoropiperidin-4-yl)methoxy)-3-nitrobenzenesulfonamide | HCID 67126502 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-((1-(1,3-Difluoropropan-2-yl)-4-fluoropiperidin-4-yl)methoxy)-3-nitrobenzenesulfonamide | HCID 67422931 | — |
反応手順
To a suspension of EXAMPLE 341C (0.100 g) and 1,3-difluoropropan-2-one (0.025 g) in dichloromethane (2 mL) was added sodium triacetoxyborohydride (0.071 g). After 15 minutes, N,N-dimethylformamide was added dropwise until an orange solution resulted (−15 drops). After stirring overnight additional 1,3-difluoropropan-2-one and sodium triacetoxyborohydride were added. After 3 hours, the reaction was loaded onto silica gel (Reveleris 40 g) and eluted with a gradient of 0.5-5% methanol/dichloromethane over 30 minutes (flow=40 ml/minutes) to provide the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09029404B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-16aaffaa1c0345aea03d2c6139ed2bc1 |
| 出典メモ | uspto-grants-2015_05 |