تفاعل #53850

ord-6f77e3edc53c475a86f94454093a89b1

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزThe mixture was concentrated under vacuum
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in saturated NaHCO3/Et2O(3×)
  3. 3
    غسيلThe organic phases were washed with brine
  4. 4
    تجفيفdried over Na2SO4
  5. 5
    أخرىevaporated

الإجراء التجريبي

To 1.72 g (4.58 mmol) trans-Methanesulfonic acid 4-[(4-chloro-phenoxycarbonyl)-methyl-amino]-cyclohexylmethyl ester in 17 ml DMF, 0.78 g (6.86 mmol, 1.5 eq) potassium thioacetate were added and the mixture was heated to 100° C. for 10 min. The mixture was concentrated under vacuum and the residue was dissolved in saturated NaHCO3/Et2O(3×). The organic phases were washed with brine, dried over Na2SO4 and evaporated to yield 1.69 g (quantitative) of trans-Thioacetic acid S-{4-[(4-chloro-phenoxycarbonyl)-methyl-amino]-cyclohexylmethyl} ester, MS: 356 (MH+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06858651B2uspto-grants-2005_02