Diethyl Ether → Acetic acid 2-chloromethoxy-ethyl ester

Temperatur

23 °C

A 5 L three-neck flask was fitted with mechanical stirrer, thermometer, 500 mL additional funnel and argon purged. 1,3-Dioxalane (140 mL, 2.00 mol) in anhydrous Et2O (800 mL) and 1.0 M ZnCl2/Et2O (7.5 mL, 0.007 mol) were added. A solution of acetyl chloride (157 mL, 2.20 mol) in Et2O (200 mL) was added dropwise through an additional funnel over 20 min. A cold water bath was used to maintain temperature between 19-27° C. throughout. Continue stirring without external cooling for 4 h, reaction self heating at 20-25° C. for about 1 h. A clear, colorless solution retained under argon overnight. Stood for 3 days and formed an orange solution. Strip Et2O on rotavap (water aspirator) until no more distilled at 35° C. bath. A quantitative yield of product 318 g (theoretical yield 306 g) was obtained.

1. customA 5 L three-neck flask was fitted with mechanical stirrer
2. customthermometer, 500 mL additional funnel and argon purged
3. customA cold water bath was used
4. temperaturewithout external cooling for 4 h
5. customreaction self
6. temperatureheating at 20-25° C. for about 1 h
7. waitStood for 3 days
8. customformed an orange solution
9. distillationStrip Et2O on rotavap (water aspirator) until no more distilled at 35° C. bath

ORD-Eintrag

ord-d8b12e2b0da34609a9e3acd890a30150

Quelldatensatz

uspto-grants-2009_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07553825B2