1,2-Dichloroethane → {2-(4-Hydroxy-phenyl)-1-[1-methylcarbamoyl-2-(4-nitro-phenyl)-ethylcarbamoyl]-ethyl} carbamic acid tert-butyl ester

関与物質

役割	名称	HCID	仕込み量
反応物	1,2-Dichloroethane	HCID 11	—
反応物	Water	HCID 962	—
反応物	Dimethylformamide	HCID 6228	—
反応物	1-Hydroxybenzotriazole	HCID 75771	—
反応物	Diisopropylethylamine	HCID 81531	—
反応物	L-Tyrosine, N-(1,1-dimethylethoxy)carbonyl-	HCID 117439	—
生成物	{2-(4-Hydroxy-phenyl)-1-[1-methylcarbamoyl-2-(4-nitro-phenyl)-ethylcarbamoyl]-ethyl} carbamic acid tert-butyl ester	HCID 68657947	—

反応手順

H-L-Phe(4-NO2)—NMe (200 mg, 0.770 mmol) is dissolved in 1 mL DMF. Diisopropylethylamine (209 mg, 1.62 mmol), EDC (162 mg, 0.847 mmol), HOBt.H2O (130 mg, 0.847 mmol), and Boc-Tyr (238 mg, 0.847 mmol) are added and the mixture is stirred for 18 hr. at 20° C. The mixture is partitioned between water and EtOAc (2×60 mL). The organics are combined and washed with brine, dried over MgSO4, filtered and evaporated to give crude product. Purification by flash chromatography, which is eluted with 97:3 DCM:methanol to give pure white solid.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07769575B2
出典データセット	uspto-grants-2010_08
ORD ID	ord-08d5b3304b664301be4a5410300acdb9
出典メモ	uspto-grants-2010_08