関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-(Bromomethyl)-5-(trifluoromethyl)benzonitrile | HCID 11601369 | — |
| 反応物 | Ammonia methanol | HCID 21705897 | — |
| 生成物 | 3-(Aminomethyl)-5-(trifluoromethyl)benzonitrile | HCID 45115840 | — |
反応手順
3-Bromomethyl-5-trifluoromethyl-benzonitrile (which is prepared in Reference Example 12) (15.9 g) is dissolved in 7M-ammonia/methanol (550 ml), and the mixture is stirred at 50-60° C. for 30 minutes. The reaction solution is concentrated under reduced pressure. To the resulting residue are added a saturated aqueous sodium bicarbonate solution and chloroform, and the mixture is separated, and the organic layer is dried over sodium sulfate, and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (chloroform:methanol=1:0→19:1→chloroform:methanol:ammonium hydroxide solution=19:1:0.1) to give 3-aminomethyl-5-trifluorometyl-benzonitrile (10.4 g). MS (m/z): 201 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08076364B2 |
|---|
| 出典データセット | uspto-grants-2011_12 |
|---|
| ORD ID | ord-59a4312b22d24405804e93c91807a522 |
|---|
| 出典メモ | uspto-grants-2011_12 |
|---|