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

反応式

[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]

参加物

反応物 2

HCID 531671-Methylpiperazine

HCID 547815Methyl isocyanoacetate

生成物 1

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

実験手順

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).

後処理

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

出典と根拠

ORDレコード: ord-dd4134985667492ab88b59d1c0e34cd9
出典データセット: uspto-grants-2012_10
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08288556B2

反応ノート

読み込み中…

参加物