Reaktion #608484

Reaktionsgleichung

1,2-bis(trimethylsilyloxy)ethane

4,4-dimethyl-5-nitropentan-2-one

→

2-(2,2-dimethyl-3-nitropropyl)-2-methyl-[1,3]dioxolane

Ausbeute 97.2%

Lösungsmittel

dichloromethane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe cooling bath was removed
2. 2
   FiltrationThe solution was filtered through a plug of potassium carbonate
3. 3
   Einengenconcentrated under reduced pressure

Vorschrift

A stirred solution of 1,2-bis(trimethylsilyloxy)ethane (26.5 g, 128 mmol) in dichloromethane (50 mL) was cooled in a dry ice/isopropanol bath, and trimethylsilyl trifluoromethanesulfonate (2.2 g, 1.0 mmol) was added, followed by the dichloromethane solution of 4,4-dimethyl-5-nitropentan-2-one (50 mL, 19.0 g, 119 mmol) from the previous step. After 30 minutes, the cooling bath was removed and the solution was allowed to warm to room temperature. The solution was filtered through a plug of potassium carbonate and concentrated under reduced pressure to provide 2-(2,2-dimethyl-3-nitropropyl)-2-methyl-[1,3]dioxolane (23.5 g) as a dark oil that was used directly in the next step without further purification.

Quelle