tert-butyl N-(4-aminobutyl)carbamate → HCID 68186050、化合物

A mixture of [(4S)-6-(4-chlorophenyl)-1-methyl-8-(methyloxy)-4H-[1,2,4]triazolo[4,3-a][1,4]benzodiazepin-4-yl]acetic acid (for a preparation see Reference compound H) (1.0 g, 2.5 mmol), HATU (1.9 g, 5 mmol) and DIPEA (0.88 ml, 5 mmol) was stirred for 80 minutes at room temperature, to this was added 1,1-dimethylethyl (4-aminobutyl)carbamate (1.05 ml, 5.0 mmol, available from Aldrich). The reaction mixture was stirred at room temperature for 2 h before it was concentrated. The residue was taken up in dichloromethane and washed with 1N HCl. The aqueous layer was extracted with dichloromethane twice. Organic layer was washed with 1N sodium hydroxide, followed by a saturated solution of sodium chloride, dried over sodium sulphate and concentrated. The residue was purified by flash-chromatography on silica using dichloromethane/methanol 95/5 to give the title compound as a yellow solid (1.2 g). LC/MS (Method A): rt=3.04 min.

1. stirringThe reaction mixture was stirred at room temperature for 2 h before it
2. concentrationwas concentrated
3. washwashed with 1N HCl
4. extractionThe aqueous layer was extracted with dichloromethane twice
5. washOrganic layer was washed with 1N sodium hydroxide
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated
8. customThe residue was purified by flash-chromatography on silica

ORDレコード

ord-26f35b5265d54dc2bda976b9aafe9a05

出典データセット

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09085582B2