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Aluminium lithium hydride → N-Methyl-N-[(1-methyl-1H-indazol-3-yl)methyl]amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | N,1-dimethyl-1H-indazole-3-carboxamide | HCID 22593809 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-Methyl-N-[(1-methyl-1H-indazol-3-yl)methyl]amine | HCID 7537473 | 104% |
反応手順
To a solution of N,1-dimethyl-1H-indazole-3-carboxamide (3.42 g, 18 mmole) in dry THF (90 mL) was added a solution of LiAlH4 in THF (1.0 M, 36 mL, 36 mmole) slowly at RT. After 2 hr the mixture was heated to a gentle reflux. After 4 hr the mixture was cooled to RT and quenched by dropwise addition of 2.0 M NaOH until a white solid had formed. The mixture was dried (MgSO4), filtered, and concentrated under reduced pressure to give the title compound (3.28 g, 100%) as an oil which was sufficiently pure for use in the next step: MS (ES) m/e 176 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07790716B2 |
| 出典データセット | uspto-grants-2010_09 |
| ORD ID | ord-c101ae9b67364dc3a978e0c2625cde97 |
| 出典メモ | uspto-grants-2010_09 |