تفاعل #835702

ord-f0ae60bf2444428eab492819cf7c222d

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصfollowed by the extraction with aqueous HCl (5%)
  2. 2
    استخلاصextracted with methylene chloride
  3. 3
    تجفيفThe organic phase was dried (Na2SO4)
  4. 4
    أخرىevaporated in vacuo

الإجراء التجريبي

To a solution of N′-ethyl-N,N-dimethylethane-1,2-diamine (0.62 mL, 4.4 mmol) in methylene chloride (10 mL) was added 6-chloropyridine-3-sulfonylchloride (0.85 g, 4 mmol; described in: Naegeli, C. et al. Helv. Chim. Actal. 1938, 21, 1746-1750) dissolved in methylene chloride (10 mL) dropwise. The reaction mixture was stirred for 30 min at room temperature followed by the extraction with aqueous HCl (5%). The acidic water layer was alkalized with an aqueous saturated solution of NaHCO3 and extracted with methylene chloride. The organic phase was dried (Na2SO4) and evaporated in vacuo to give 0.7 gram (60% yield) of the title compound: MS (ES) m/z 292 (M++1).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07399780B2uspto-grants-2008_07