関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | methyl N-[(3'-cyanobiphenyl-4-yl)sulfonyl]valinate | HCID 66769160 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | methyl N-{[3'-(aminomethyl)biphenyl-4-yl]sulfonyl}valinate | HCID 66769176 | 76% |
反応手順
A suspension of methyl N-[(3′-cyanobiphenyl-4-yl)sulfonyl]valinate obtained in Reference Example 93 (5.00 g, 13.4 mmol), Raney-nickel (5.00 g) and 28% aqueous ammonia (50 mL) in THF (50 ml)-methanol (50 mL) was stirred at room temperature for 15 hr under hydrogen atmosphere (1 atm). The catalyst was filtered off, and the filtrate was concentrated under reduced pressure. A mixed solvent of ethyl acetate-hexane was added to the residue, and the precipitated insoluble material was filtered off. The filtrate was washed with saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, and diethyl ether was added to the residue. The precipitated solid was collected by filtration to give the title compound as a white powder (3.84 g, 76%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07915267B2 |
|---|
| 出典データセット | uspto-grants-2011_03 |
|---|
| ORD ID | ord-0aec9decdc4540d6b8cd8466e00d937a |
|---|
| 出典メモ | uspto-grants-2011_03 |
|---|