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N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethyl]amine → N,N-dimethyl-N-[2-(7-amino-1H-indazol-4-yl)ethyl]amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethyl]amine | HCID 13629307 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N,N-dimethyl-N-[2-(7-amino-1H-indazol-4-yl)ethyl]amine | HCID 13629325 | 82.2% |
反応手順
In the presence of 1.0 g of Raney nickel, 1.2 g of N,N-dimethyl-N-[2-(7-nitro-1H-indazol-4-yl)ethyl]amine is hydrogenated in 60 ml of tetrahydrofuran. The mixture is filtered, concentrated and recrystallized from ethyl acetate/hexane, thus producing 860 mg of N,N-dimethyl-N-[2-(7-amino-1H-indazol-4-yl)ethyl]amine, mp 125° C. This product is treated, in the amount of 460 mg, with ethanol and ethereal hydrochloric acid, recrystallization from methanol/diethyl ether yielding 505 mg of N,N-dimethyl-N-[2-(7-amino-1H-indazol-4-yl)ethyl]amine, dihydrochloride, mp 231°-232° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04958026 |
| 出典データセット | uspto-grants-1990_09 |
| ORD ID | ord-3146ba50f27c4b099d0409cdbd648f63 |
| 出典メモ | uspto-grants-1990_09 |