Dichloromethane → 23946-74-9

Temperatur

0 °C

A solution of 1-methoxy-2-propanol in dichloromethane (2.3 g, 25.5 mmol) (25 ml) and pyridine (5 ml) was cooled to between −5 and 0° C. 4-Methylbenzenesulfonyl chloride (5.35 g, 28.1 mmol) was added dropwise and the mixture was stirred at 0° C. for 15 minutes. The mixture was then stirred at room temperature for 18 hours. Ice was added and the mixture was stirred for 1 hour. The organic phase was separated, washed with 10% aqueous sulfuric acid (4×) and water (1×), and then dried (MgSO4) and filtered. The filtrate was purified by column chromatography on silica gel eluting with dichloromethane. The solution obtained was dried (MgSO4), filtered, and concentrated under reduced pressure to afford the title compound as a colorless oil, 4.3 g, 69% yield.

1. stirringThe mixture was then stirred at room temperature for 18 hours
2. additionIce was added
3. stirringthe mixture was stirred for 1 hour
4. customThe organic phase was separated
5. washwashed with 10% aqueous sulfuric acid (4×) and water (1×)
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customThe filtrate was purified by column chromatography on silica gel eluting with dichloromethane
9. customThe solution obtained
10. dry with materialwas dried (MgSO4)
11. filtrationfiltered
12. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-00ac4b5901094b7993766dee5e494c60

Quelldatensatz

uspto-grants-2005_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06949577B2