Triethylamine → t-butyl 2-[[3-(5H-dibenzo[a,d][7]annulen-5-ylidene)propyl](methyl)amino]-2-oxoethylcarbamate

105 mg (0.60 mmol) of t-butoxycarbonylglycine, 111 mg (0.58 mmol) of 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide hydrochloride, 133 mg (0.51 mmol) of 3-(5H-dibenzo[a,d][7]annulen-5-ylidene)-N-methyl-1-propanamine and 0.08 ml (0.57 mmol) of triethylamine were stirred in 5 ml of dichloromethane at room temperature overnight. Saturated aqueous sodium hydrogencarbonate solution was added to the reaction mixture. After extracting with dichloromethane, the organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by the silica gel chromatography (hexane:ethyl acetate=2:1) to obtain the title compound.

1. extractionAfter extracting with dichloromethane
2. dry with materialthe organic layer was dried over anhydrous sodium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by the silica gel chromatography (hexane:ethyl acetate=2:1)

ORDレコード

ord-9a636358df0643fea0f175198e3beaf4

出典データセット

uspto-grants-2012_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08278329B2