1,1'-Carbonyldiimidazole → HCID 59909822, Verbindung

A solution of (2R)-2-[2-(tert-butoxy)-2-oxoethyl]-5-cyclohexylpentanoic acid (Preparation 1) (300 mg, 1.00 mmol) in dichloromethane (15 ml) was treated with 1,1′-carbonyldiimidazole (162 mg, 1.00 mmol) and the solution was stirred at room temperature for 2 hours. N-hydroxy-2-(phenylsulfonyl)ethanimidamide (J.Heterocycl.Chem.; 16; 1979; 1197-1200) (214 mg, 1.00 mmol) was then added and the mixture was stirred for 17 hours. The solvent was removed under reduced pressure and the residue was heated neat at 130° C. under a nitrogen atmosphere for 2 hours. The crude product was then purified by column chromatography on silica gel eluting with dichloromethane:methanol (99:1) to afford the title compound (78 mg).

1. stirringthe mixture was stirred for 17 hours
2. customThe solvent was removed under reduced pressure
3. temperaturethe residue was heated neat at 130° C. under a nitrogen atmosphere for 2 hours
4. customThe crude product was then purified by column chromatography on silica gel eluting with dichloromethane:methanol (99:1)

ORD-Eintrag

ord-c283a2629b434db3a41566e06a79f14d

Quelldatensatz

uspto-grants-2005_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06897306B2