Triethylamine → 1-(4-Methylpiperazin-1-yl)pent-4-yn-1-one

HRID 1984074

반응식

HRID 1984074 반응식
[C:1]([OH:7])(=O)[CH2:2][CH2:3][C:4]#[CH:5].CCN(CC)CC.ClC(OCC)=O.[CH3:21][N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1>C(Cl)Cl>[CH3:21][N:22]1[CH2:27][CH2:26][N:25]([C:1](=[O:7])[CH2:2][CH2:3][C:4]#[CH:5])[CH2:24][CH2:23]1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 224644-Pentynoic acidHCID 531671-Methylpiperazine

생성물 1

HCID 577138121-(4-Methylpiperazin-1-yl)pent-4-yn-1-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 4-pentynoic acid (519 mg, 5.29 mmol) and Et3N (737 μL, 5.29 mmol) in DCM (10 mL) was treated with ethyl chloroformate (504 μL, 5.29 mmol) at rt for 15 min. Then N-methyl-piperazine (588 μL, 5.29 mmol) was added, and stirring was prolonged for 45 min. Work-up (sat. aq. NaHCO3) and concentration gave the title compound as a colorless oil. 1H NMR (CDCl3) δ 3.63 (t, 2H), 3.48 (t, 2H), 2.55 (m, 4H), 2.38 (quint., 4H), 2.30 (s, 3H).

후처리

  1. concentration(sat. aq. NaHCO3) and concentration

출처 및 근거

ORD 기록
ord-4251d02f6efa41f88dd90cc28264d645
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07544672B2

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