Diisopropylethylamine → Rac-4-(2-iodo-5-methanesulfonyl-benzoyl)-3-methyl-piperazine-1-carboxylic acid tert-butyl ester

참여 물질

역할	이름	HCID	투입량
반응물	Diisopropylethylamine	HCID 81531	—
반응물	O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate	HCID 2733207	—
반응물	tert-Butyl 3-methylpiperazine-1-carboxylate	HCID 2756810	—
반응물	2-Iodo-5-methanesulfonyl-benzoic acid	HCID 57445281	—
용매	Dimethylformamide	HCID 6228	—
생성물	Rac-4-(2-iodo-5-methanesulfonyl-benzoyl)-3-methyl-piperazine-1-carboxylic acid tert-butyl ester	HCID 59793735	47.1%

반응 단계

To a solution of rac-3-Methyl-piperazine-1-carboxylic acid tert-butyl ester (350 mg, 1.75 mmol) in dimethylformamide (3 ml) were added 2-Iodo-5-methanesulfonyl-benzoic acid (540 mg, 1.67 mmol), N-ethyldiisopropylamine (1.8 ml, 10.5 mmol), and TBTU (630 mg, 1.92 mmol). The reaction mixture was then allowed to stir at room temperature for 16 hours. The reaction mixture was then concentrated in vacuo and the residue was purified by column chromatography (SiO2, 20 g, Heptane/EtOAc 0-100%) to give the title compound (400 mg, 45%). MS (m/e): 526.2 (M+NH4+).

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US07427612B2
출처 데이터셋	uspto-grants-2008_09
ORD ID	ord-edf9f4fdab1941119255d8969f0c13db
출처 메모	uspto-grants-2008_09