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Sodium Hydroxide → N-[5-bromo-6-chloro-2-(4-cyanophenylamino)-pyrimidin-4-yl]benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | N-Bromosuccinamide | HCID 9834204 | — |
| 反応物 | N-[6-chloro-2-(4-cyanophenylamino)pyrimidin-4-yl]benzamide | HCID 71465002 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[5-bromo-6-chloro-2-(4-cyanophenylamino)-pyrimidin-4-yl]benzamide | HCID 71465003 | — |
反応手順
1000 ml of dichloromethane and 100 g of N-[6-chloro-2-(4-cyanophenylamino)pyrimidin-4-yl]benzamide were added to a reaction vessel. To this was added 76.5 g of N-bromosuccinamide and 2.2 g (10M %) of ammonium acetate and stirred for 4 hrs. After completion of the reaction, the pH was adjusted to 10-11 with 5% of aqueous sodium hydroxide solution (10 g in 200 ml water). The reaction mass was filtered and the wet cake was slurried in 1000 ml of hot water at 55-60° C. for 1 hr and filtered. The obtained solid was dried under vacuum (0.5 kg/cm2) at 55-60° C. overnight.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653266B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-f10d23cf54844123b63e6a5067e0870a |
| 出典メモ | uspto-grants-2014_02 |