Trimethyl orthoformate → (2,2-Bis(fluoromethyl)-1,3-dioxan-5-yl)methanol

Temperatur

60 °C

A mixture of 2-(hydroxymethyl)-1,3-propanediol (2.2 g, 20.7 mmol), 1,3-difluoroacetone (3.89 g, 41.4 mmol), trimethyl orthoformate (3.44 ml, 20.7 mmol), and p-toluenesulfonic acid monohydrate (356 mg, 2.07 mmol) was stirred at 60° C. for 10 hours. After completion of the reaction, triethylamine (577 μl) was added to the reaction mixture, which was then concentrated. The residue was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate) to obtain the title compound (1.6 g, yield: 43.4%) as a light yellow oil.

1. additionwas added to the reaction mixture, which
2. concentrationwas then concentrated
3. customThe residue was purified by silica gel column chromatography (elution solvent: heptane/ethyl acetate)

ORD-Eintrag

ord-643f1dd86f91404aa5f5e314bc0f49bb

Quelldatensatz

uspto-grants-2008_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07425634B2