반응 #8519

ord-1dafe2e64013446290804c2d6d9417a2

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITAfter one hour
  2. 2
    기타all the volatile components were removed under reduced pressure
  3. 3
    세척washed twice with 100 ml of water each time
  4. 4
    기타dried
  5. 5
    기타evaporated under reduced pressure

실험 절차

1.83 g (19 mmol) of sodium t-butoxide and 2.78 g (19 mmol) of octanethiol were stirred into 40 g of methanol at room temperature. After 30 minutes, the clear solution was added in one portion to 3.33 g (19 mmol) of p-xylylene dichloride in 100 g of methanol. After one hour, the mixture was neutralized using 1N hydrochloric acid, and all the volatile components were removed under reduced pressure. The crude product was taken up in 250 ml of chloroform and washed twice with 100 ml of water each time, dried and evaporated under reduced pressure. 5.29 g, which, according to 1H-NMR-spectroscopy, consisted of 50% of product, 25% of starting material and 25% of p-bis(octylthiomethyl)benzene.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087787B1uspto-grants-2006_08