Dichloromethane → Di[(2E,4E,6E,8E)-3,7-dimethyl-9-(2,6,6-trimethyl-1-cyclohexenyl)-2,4,6,8-nonatetraenyl](2S)-2-[(tert-butoxycarbonyl)amino]butanedioate

참여 물질

역할	이름	HCID	투입량
반응물	Dichloromethane	HCID 6344	—
반응물	N-(tert-butoxycarbonyl)-L-aspartic acid	HCID 99718	—
반응물	Retinol	HCID 445354	—
반응물	1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride	HCID 2723939	—
용매	Dimethylformamide	HCID 6228	—
생성물	Di[(2E,4E,6E,8E)-3,7-dimethyl-9-(2,6,6-trimethyl-1-cyclohexenyl)-2,4,6,8-nonatetraenyl](2S)-2-[(tert-butoxycarbonyl)amino]butanedioate	HCID 86590977	—

반응 조건

온도	0 °C

반응 단계

N-Boc aspartic acid (1.2 mg), methylene chloride 20 ml and minimum amount of dimethylformamide (DMF) were added to nitrogen filled, three mouth- round bottom flask and melted. The reaction mixture was cooled down into 0° C., 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride [EDCI](1.36 g)were added slowly, and stirred for approximately 30 minutes. Retinol (0.51 g) was added into the reaction mixture, small amount of N,N′-dimethylaminopyridine (DMAP) were added immediately, and stirred for approximately 1˜3 hours. After the reaction was finished, eluent were removed under the low pressure, the residues were melted with ethyl acetate and washed several times with water and Brine. Organic phase were dried with anhydrous MgSO4, concentrated under low pressure and separated with column chromatography.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US07030265B2
출처 데이터셋	uspto-grants-2006_04
ORD ID	ord-cf1da0af55b84698803c304c84df7561
출처 메모	uspto-grants-2006_04