반응 #59874

반응 방정식

2-(hydroxymethyl)-1,3-propanediol

1,3-difluoroacetone

trimethyl orthoformate

p-toluenesulfonic acid monohydrate

→

title compound

수율 43.4%

(2,2-bis(fluoromethyl)-1,3-dioxan-5-yl)methanol

수율 43.4%

용매

triethylamine

반응 조건

후처리

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

실험 절차

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.

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