تفاعل #80967

ord-a7eb556908204482bceb93a605ec7ad7

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةat reflux for 3.5 h
  3. 3
    درجة الحرارةto cool
  4. 4
    ترشيحfiltered
  5. 5
    أخرىthe solvent was removed in vacuo

الإجراء التجريبي

A mixture of 94.0 g (0.91 mol) of 2-methylpropane-thioamide, 115.7 g (0.91 mol) of 1,3-dichloroacetone, and 109.7 g (0.91 mol) of MgSO4 in 1.6 liters of acetone was heated at reflux for 3.5 h. The resulting mixture was allowed to cool, filtered, and the solvent was removed in vacuo to provide the crude desired compound as a yellow oil. 1H NMR (DMSO-d6) δ1.32 (d, J=7 Hz, 6H), 3.27 (heptet, J=7 Hz, 1H), 4.78 (s, 2H), 7.61 (s, 1H). Mass spectrum: (M+H)+ =176.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05616720uspto-grants-1997_04