Piperazine → Trifluoroacetylpiperazine
反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C([O:9][C:10](=O)[C:11]([F:14])([F:13])[F:12])C>CO>[F:12][C:11]([F:14])([F:13])[C:10]([N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)=[O:9]参加物
4
実験手順
To a solution of piperazine (1.444 g, 16.8 mmol) in MeOH (10 mL) was added trifluroacetic acid ethyl ester (2.0 mL, 16.8 mmol) and the mixture stirred at room temperature overnight. The reaction was concentrated and purified by column chromatography on silica gel (CH2Cl2/MeOH, 9:1) to afford the desired mono-protected piperazine adduct (1.77 g, 58%) as a pale yellow oil. 1H NMR (CDCl3) δ 1.70 (br s, 1H), 2.90–2.94 (m, 4H), 3.56–3.59 (m, 2H), 3.64–3.67 (m, 2H).
後処理
- concentrationThe reaction was concentrated
- custompurified by column chromatography on silica gel (CH2Cl2/MeOH, 9:1)
出典と根拠
- ORDレコード
- ord-214ef05a35294d9a86a8c36032007d91
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091217B2
反応ノート
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