1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 58116824、化合物

関与物質

役割	名称	HCID	仕込み量
反応物	1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide	HCID 15908	—
反応物	Diisopropylethylamine	HCID 81531	—
反応物	n,n-Dimethylpiperazine-1-carboxamide	HCID 712909	—
反応物	4-Bromocrotonic acid	HCID 6436411	—
反応物	(3,4-Dichloro-phenyl)-(5,6,7,8-tetrahydro-9-thia-1,3,7-triaza-fluoren-4-yl)-amine	HCID 58116912	—
溶媒	Water	HCID 962	—
溶媒	Dichloromethane	HCID 6344	—
生成物	HCID 58116824	HCID 58116824	24%

反応手順

(2E)-4-Bromobut-2-enoic acid (106 mg, 0.64 mmol) and piperazine-1-carboxylic acid dimethylamide (107 mg, 0.68 mmol) were dissolved in DCM (5.0 mL), and DIPEA (111 mg, 0.85 mmol) was added. The mixture was stirred at rt for 2 h. Subsequently, the compound from Example 15A (150 mg, 0.43 mmol), DIPEA (55 mg, 0.43 mmol) and EDCI (82 mg, 0.43 mmol) were added. The reaction mixture was stirred at rt overnight. Then, water was added, and the mixture was extracted three times with DCM. The combined organic layers were dried over sodium sulfate. The solvent was removed in vacuo, and the residue was purified by preparative HPLC to yield 59 mg (24%) of the title compound.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08524722B2
出典データセット	uspto-grants-2013_09
ORD ID	ord-3db0a56a8e02415888246276a89874c5
出典メモ	uspto-grants-2013_09