Hydrochloric Acid → HCID 67593614, Verbindung

Temperatur

-78 °C

The compound from Step 3 (1.03 g, 5.0 mmol) was dissolved in tetrahydrofuran (50 mL) and cooled to -78° C. A solution of sodium bistrimethylsilylamide (5.0 mL of a 1.0M tetrahydrofuran solution) was added and the reaction stirred for 0.75 hours at -78° C. Trifluoroacetyl imidazole (0.68 mL, 6.0 mmol) was added and the reaction was warmed to room temperature and stirred under a nitrogen atmosphere for 16 hours. At this time, 1N hydrochloric acid (300 mL) was added to the reaction followed by extraction with ether (350 mL). The organics were washed with brine (200 mL), dried over MgSO4 and concentrated in vacuo. The resulting yellow oil was used without further purification.

1. temperaturethe reaction was warmed to room temperature
2. stirringstirred under a nitrogen atmosphere for 16 hours
3. extractionfollowed by extraction with ether (350 mL)
4. washThe organics were washed with brine (200 mL)
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. customThe resulting yellow oil was used without further purification

ORD-Eintrag

ord-f2b1a608cc5949009b328aed1aea301f

Quelldatensatz

uspto-grants-1996_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05547975