Piperazine → Trifluoroacetylpiperazine

HRID 8932

反応式

HRID 8932 の反応式
[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

反応物 2

HCID 4837PiperazineHCID 9794Ethyl trifluoroacetate

生成物 1

HCID 7172020Trifluoroacetylpiperazine収率 58%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

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

  1. concentrationThe reaction was concentrated
  2. 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

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