Triethylamine → HCID 68703339, Verbindung

A solution of 2-(4-chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-ethanone (4.5 g, 87% pure, 13.85 mmol) and triethylamine (1.7 g, 2.35 ml, 16.8 mmol, 1.2 eq.) in methylene chloride (100 ml) is treated dropwise at ambient temperature with isobutyryl chloride (1.79 g, 1.76 ml, 16.8 mmol, 1.2 eq.). After stirring for 5 h, the solution is washed successively with 2M HCl solution and saturated sodium hydrogen carbonate solution. The organic phase is dried over anhydrous magnesium sulphate, filtered and evaporated to dryness in vacuo to afford a black residue. This is triturated with methanol at room temperature overnight to afford a brown solid, which is filtered and washed with methanol. The solid is purified twice by flash chromatography (ethyl acetate/cyclohexane=1:9) to furnish the title compound.

1. washthe solution is washed successively with 2M HCl solution and saturated sodium hydrogen carbonate solution
2. dry with materialThe organic phase is dried over anhydrous magnesium sulphate
3. filtrationfiltered
4. customevaporated to dryness in vacuo
5. customto afford a black residue
6. customThis is triturated with methanol at room temperature overnight
7. customto afford a brown solid, which
8. filtrationis filtered
9. washwashed with methanol
10. customThe solid is purified twice by flash chromatography (ethyl acetate/cyclohexane=1:9)

ORD-Eintrag

ord-1a5857e3db8c41c8b57535852103d956

Quelldatensatz

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07732435B2