Methyl iodide → HCID 22277998, Verbindung

In a 100 mL round bottom flask, was added 0.4 g 1-Cyclohexylmethyl-4-(3,4-dichloro-phenyl)-5-pyridin-4-yl-pyrazolidin-3-one and 20 mL THF, stirred at 0° C. under nitrogen. 1.32 mL 1 M LHMDS in THF was added drop wise. After stirred at 0° C. for 30 min. 0.11 mL iodomethane was added drop wise. The resulted mixture was stirred from 0° C. to rt for 2 hour, quenched with 50 mL sat. NH4Cl, extracted with dichloromethane 3×25 mL. The organic phase was dried over anhydrous Na2SO4. After purification by flash chromatography, obtained the title compound 0.4 g as light solid. MS (ES+): 418 (M+H)+.

1. stirringAfter stirred at 0° C. for 30 min
2. stirringThe resulted mixture was stirred from 0° C. to rt for 2 hour
3. customquenched with 50 mL sat. NH4Cl
4. extractionextracted with dichloromethane 3×25 mL
5. dry with materialThe organic phase was dried over anhydrous Na2SO4
6. customAfter purification by flash chromatography

ORD-Eintrag

ord-010f13a294ec41b9969f3b6adeab9adb

Quelldatensatz

uspto-grants-2005_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06967254B2