2,6-Lutidine → HCID 18993077, Verbindung

To a 0° C. solution of 5-hydroxymethyl-2-carboethoxyfuran (2.94 g, 17.3 mmol), prepared as in step 1, in CH2Cl2 (50 mL) was added 2,6-lutidine (2.50 mL, 21.5 mmol) and methanesulfonyl chloride (1.50 mL, 19.0 mmol). The reaction mixture was stirred for 40 min at 0° C., then the cold bath was removed and stirring was continued for 2 hours. The reaction mixture was extracted with 1N aqueous HCl and saturated aqueous NaHCO3, and the organic phase was dried over MgSO4, filtered, and concentrated in vacuo to give 5-methanesulfonyloxymethyl-2-carboethoxyfuran (4.0 g) as a yellow oil which was used without further purification.

1. customthe cold bath was removed
2. stirringstirring
3. waitwas continued for 2 hours
4. extractionThe reaction mixture was extracted with 1N aqueous HCl and saturated aqueous NaHCO3
5. dry with materialthe organic phase was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo

ORD-Eintrag

ord-167a3b83373c4a7fa6b1e59df3d5e89d

Quelldatensatz

uspto-grants-1996_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05486525