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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1060426Generated: October 25, 2026

Methyl isothiocyanate → N-[2-chloro-4-(3-methylthioureido)benzoyl]-4-(2-methoxyphenyl)-L-phenylalanine methyl ester

https://huagongshe.com/reaction/1060426

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethyl isothiocyanateHCID 11167—
ReactantDiisopropylethylamineHCID 81531—
ReactantN-(4-amino-2-chlorobenzoyl)-4-(2-methoxyphenyl)-L-phenylalanine methyl esterHCID 54392214—
Catalyst4-(Dimethylamino)pyridineHCID 14284—
SolventDimethylformamideHCID 6228—
SolventEthyl AcetateHCID 8857—
ProductN-[2-chloro-4-(3-methylthioureido)benzoyl]-4-(2-methoxyphenyl)-L-phenylalanine methyl esterHCID 54405488—

Reaction Conditions

Temperature90 °C

Reaction Steps

Methylisothiocyanate (43 μL) was added to a solution of N-(4-amino-2-chlorobenzoyl)-4-(2-methoxyphenyl)-L-phenylalanine methyl ester (55.1 mg) in anhydrous DMF (1 mL) containing DIEA (22 μL) and DMAP (catalitic amount). The resulting mixture was then heated at 90° C. under N2 for 1 d. After cooling, the mixture was diluted with EtOAc, washed sequentially with 1N HCl, satd. NaHCO3 and water, dried (MgSO4) and evaporated. The residue was purified by preparative TLC (silica gel) using CH2Cl2/MeOH (15:1) as an eluent to give N-[2-chloro-4-(3-methylthioureido)benzoyl]-4-(2-methoxyphenyl)-L-phenylalanine methyl ester (22.7 mg). ESMS: m/z 512 (MH+).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06521666B1
Source datasetuspto-grants-2003_02
ORD IDord-358f1c936d364d5e8ed4ccaf1863b67c
Source noteuspto-grants-2003_02