Reaktion #68038

Reaktionsgleichung

chloroform

(2,2-difluorobenzo[1,3]dioxol-5-yl)methanol

→

2,2-difluorobenzo[1,3]dioxol-5-carbaldehyde

Lösungsmittel

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe insoluble material filtered off
2. 2
   Sonstigethe solvent was removed under reduced pressure
3. 3
   SonstigeThe residue thus obtained
4. 4
   Sonstigewas purified by silica gel column chromatography [silica gel; Silica gel 60 manufactured by Kanto Chemical Co., Inc., eluent; ethyl acetate:hexane 1:2]

Vorschrift

To 20 mL of chloroform containing 930 mg of (2,2-difluorobenzo[1,3]dioxol-5-yl)methanol and 20 mL of a tetrahydrofuran solution, 2.20 g of manganese dioxide was added, and the mixture was stirred at room temperature for 3 days. The insoluble material filtered off, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [silica gel; Silica gel 60 manufactured by Kanto Chemical Co., Inc., eluent; ethyl acetate:hexane 1:2] to obtain 687 mg of a yellow oily substance, 2,2-difluorobenzo[1,3]dioxol-5-carbaldehyde.

Quelle