Aluminium lithium hydride → 1,3,3-Trimethylpiperazine
反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].C(O[C:12]([N:14]1[CH2:19][CH2:18][NH:17][C:16]([CH3:21])([CH3:20])[C:15]1=O)=O)(C)(C)C>C1COCC1>[CH3:12][N:14]1[CH2:19][CH2:18][NH:17][C:16]([CH3:21])([CH3:20])[CH2:15]1参加物
4
反応条件
- 温度
- 50 °C
実験手順
LiAlH4 (1M in THF, 32.5 mL, 32.5 mmol, 1.5 equiv) was added to a solution of 3,3-dimethyl-2-oxo-piperazine-1-carboxylic acid tert-butyl ester (Step 114.3) (4.95 g, 21.7 mmol) in THF (100 mL) at 50° C., under an argon atmosphere. The resulting mixture was stirred for 3 h at 50° C., cooled to 0° C., quenched by addition of acetone and concentrated. The residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 94:5:1) to afford 2 g of the title compound as a yellow oil. Title compound: ESI-MS: 129.1.
後処理
- temperaturecooled to 0° C.
- customquenched by addition of acetone
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 94:5:1)
出典と根拠
- ORDレコード
- ord-d86d9ca307a3497ea7425b32fb04dc76
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08536175B2
反応ノート
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