Methyl iodide → HCID 59773514, Verbindung

Temperatur

0 °C

A solution of 1.0 eq of 96 in 30 mL of dry THF was cooled to −78° C. While stirring, 1.1 eq of n-BuLi (2.5 M in hexanes) was added dropwise. The reaction solution was warmed to 0° C. and stirred for 1 hr. The solution was then cooled to −78° C. and 1.2 eq of methyl iodide was slowly added. The mixture was stirred, as the solution warmed to rt. After 17 hrs, 50 mL of saturated NH4Cl was added and extracted with EtOAc (3×50 mL). The combined organic extracts were dried over MgSO4 and vacuum filtered. The filtrate was rotary evaporated and dried under vacuum to afford a dark orange colored solid as 97.

1. stirringstirred for 1 hr
2. temperatureThe solution was then cooled to −78° C.
3. stirringThe mixture was stirred, as the solution
4. temperaturewarmed to rt
5. extractionextracted with EtOAc (3×50 mL)
6. dry with materialThe combined organic extracts were dried over MgSO4 and vacuum
7. filtrationfiltered
8. customThe filtrate was rotary evaporated
9. customdried under vacuum
10. customto afford a dark orange colored solid as 97

ORD-Eintrag

ord-ed2fb03b0ca143c6b1f69e97269dd8fb

Quelldatensatz

uspto-grants-2008_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07417152B2