Diisopropylamine → 2-[2-(2-Methoxyethoxymethoxy)ethyl]thiophene

Temperatur

0 °C

15.0 g of 2-thiopheneethanol was dissolved in 350 mL of dichloromethane, and 30.2 g of diisopropylamine was added thereto. The resulting mixture was cooled to 0° C. and 17.5 g of 2-methoxyethoxymethyl chloride was added thereto. The resulting mixture was stirred for 2 hours and heated to reflux for 2 hours. The reaction product solution was cooled and concentrated by evaporation under reduced pressure. To the residue, 200 mL of water and 250 mL of n-hexane were added, and the resulting mixture was stirred for 5 minutes. Aqueous layer was discarded, and the organic layer was washed twice with 700 mL portions of water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 21.5 g (yield of 85%) of the title compound as a colorless oil.

1. temperatureheated
2. temperatureto reflux for 2 hours
3. temperatureThe reaction product solution was cooled
4. concentrationconcentrated by evaporation under reduced pressure
5. additionTo the residue, 200 mL of water and 250 mL of n-hexane were added
6. stirringthe resulting mixture was stirred for 5 minutes
7. washthe organic layer was washed twice with 700 mL portions of water
8. dry with materialdried over anhydrous magnesium sulfate
9. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-e81fb2b8b6d84ee4beb9aff279930772

Quelldatensatz

uspto-grants-2008_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07449580B2