1-Methylpiperazine → 2-Isocyano-1-(4-methylpiperazin-1-yl)ethanone

반응식

[N+:1]([CH2:3][C:4]([O:6]C)=O)#[C-:2].[CH3:8][N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1>>[N+:1]([CH2:3][C:4]([N:12]1[CH2:13][CH2:14][N:9]([CH3:8])[CH2:10][CH2:11]1)=[O:6])#[C-:2]

참가 물질

반응물 2

HCID 531671-Methylpiperazine

HCID 547815Methyl isocyanoacetate

생성물 1

HCID 1819132-Isocyano-1-(4-methylpiperazin-1-yl)ethanone수율 99%

실험 절차

Prepared in accordance with Method B with methyl isocyanoacetate (1.0 g, 10.09 mmol) and N-methylpiperazine (1.37 mL, 15.14 mmol). The reaction mixture was stirred overnight at RT and then concentrated. The residue was dissolved in dichloromethane (50 mL) and evaporated. The residue was coevaporated three times with a mixture of CH2Cl2:cyclohexane=50:50 (3×10 mL). After drying 2-isocyano-1-(4-methyl-piperazin-1-yl)-ethanone VIB 01128 was obtained as yellow solid (1.67 g, 99% yield).

후처리

concentrationconcentrated
dissolutionThe residue was dissolved in dichloromethane (50 mL)
customevaporated
additionwith a mixture of CH2Cl2
dry with materialAfter drying 2-isocyano-1-(4-methyl-piperazin-1-yl)-ethanone VIB 01128

출처 및 근거

ORD 기록: ord-cb1925c3ceb2463db316e217ef299eb9
출처 데이터셋: uspto-grants-2013_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08431599B2

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