Piperazine → Trifluoroacetylpiperazine

HRID 8932

반응식

HRID 8932 반응식
[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]

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 9794Ethyl trifluoroacetate

생성물 1

HCID 7172020Trifluoroacetylpiperazine수율 58%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  1. concentrationThe reaction was concentrated
  2. custompurified by column chromatography on silica gel (CH2Cl2/MeOH, 9:1)

출처 및 근거

ORD 기록
ord-214ef05a35294d9a86a8c36032007d91
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091217B2

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