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

HRID 1984074

反応式

HRID 1984074 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-4251d02f6efa41f88dd90cc28264d645
出典データセット
uspto-grants-2009_06
特許番号
US07544672B2

関連ノート

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