반응 #57999

ord-043b0c3cc51046faa4d80dcc8ff53bfc

반응 조건

온도
200°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling to ambient temperature
  2. 2
    추출extracted three times with diethyl ether
  3. 3
    세척The combined organic extracts were washed with brine
  4. 4
    건조dried (MgSO4)
  5. 5
    기타the volatiles evaporated in vacuo
  6. 6
    workup.DISTILLATIONDistillation (atmospheric pressure; ˜135° C.) of the residual liquid

실험 절차

A mixture of tert-butylamine (18.0 mL, 171 mmol) and (chloromethyl)trimethylsilane (7.00 g, 57.1 mmol) was heated in a thick-walled glass tube at 200° C. overnight. After cooling to ambient temperature, the reaction mixture was poured into 1 N NaOH and extracted three times with diethyl ether. The combined organic extracts were washed with brine, dried (MgSO4), and the volatiles evaporated in vacuo. Distillation (atmospheric pressure; ˜135° C.) of the residual liquid gave the title compound 77 as a colorless liquid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07419990B2uspto-grants-2008_09