1,4-Dioxane → 1-Cyclopropylpiperazine
反応式
[CH:1]1([N:4]2[CH2:9][CH2:8][N:7](C(OC(C)(C)C)=O)[CH2:6][CH2:5]2)[CH2:3][CH2:2]1.O1CCOCC1>Cl>[CH:1]1([N:4]2[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]2)[CH2:3][CH2:2]1参加物
4
実験手順
A solution of tert-butyl 4-cyclopropylpiperazine-1-carboxylate (0.792 g, 3.50 mmol) in 4M HCl in 1,4-dioxane (4.37 mL, 17.50 mmol) was stirred at room temperature for 3 h under nitrogen. The reaction mixture was filtered and washed with ether to afford crude 1-cyclopropylpiperazine (0.659 g) as a white solid. The crude product was purified by ion exchange chromatography, using a SCX column. The desired product was eluted from the column using 3.5M NH3/MeOH and pure fractions were evaporated to dryness to afford 1-cyclopropylpiperazine (0.264 g, 59.7%) as a yellow oil.
後処理
- filtrationThe reaction mixture was filtered
- washwashed with ether
- customto afford crude 1-cyclopropylpiperazine (0.659 g) as a white solid
- customThe crude product was purified by ion exchange chromatography
- washThe desired product was eluted from the column
- customwere evaporated to dryness
出典と根拠
- ORDレコード
- ord-7cd9b3c6ffb040d58b94fc1a4073fa4f
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737149B2
反応ノート
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