반응 #470409

ord-4447b5e2032b404f84f2158865148544

반응 방정식

[Li][CH2]CCC
BuLi
C[Si](C)(C)N[Si](C)(C)C
hexamethyldisilazane
[Cl-].[NH4+]
NH4Cl
C[Si](C)(C)[N-][Si](C)(C)C.[Li+]
lithiumhexamethyl disilazide

반응 조건

온도
-40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThe mixture subsequently stirred at −70° C. for an additional hr
  2. 2
    추출extracted with ethyl acetate

실험 절차

A solution of lithiumhexamethyl disilazide was prepared by adding 4.8 ml of 1.6 m BuLi in hexanes to a solution of 1.8 ml of hexamethyldisilazane in 10 ml of dry THF at −40° C. This solution was stirred for 15 min at −40° C. A quantity of 7.8 ml of this solution was added dropwise to a solution of 1.34 g of compound 13 in 20 ml of dry THF at −70° C. The mixture subsequently stirred at −70° C. for an additional hr and then poured into 50 ml of sat. NH4Cl solution and extracted with ethyl acetate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08367648B2uspto-grants-2013_02