تفاعل #344130

ord-9ad0605fd94a48b7bfc3e8699e18142b

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىevaporated
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in water
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    أخرىThe combined organic phases were dried
  5. 5
    أخرىevaporated
  6. 6
    أخرىThe title compound was crystallized as the oxalate salt from acetone
  7. 7
    أخرىto yield 270 mg

الإجراء التجريبي

To a solution of sodium (120 mg, 5 mmol) in 2-methoxyethanol (10 ml) was added 3-(4-chloro-1,2,5-thiadiazol-3-yl)-1,2,5,6-tetrahydro-1-methylpyridine oxalate (310 mg, 1 mmol). The mixture was stirred at 50° C. for 18 h and evaporated. The residue was dissolved in water and extracted with ethyl acetate. The combined organic phases were dried and evaporated. The title compound was crystallized as the oxalate salt from acetone to yield 270 mg. (M.p. 152.1° C.; M+ : 253; Compound 15).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05260311uspto-grants-1993_11