Реакция #156835

ord-2e44c9b0eb6d4d6dbf6b6b11b8f2d14e

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe viscous yellow reaction
  2. 2
    Температураwas heated to 90° C. for one hour
  3. 3
    Температураto cool back to room temperature
  4. 4
    Другоеpurified via column chromatography (220 g SiO2, 20-30% gradient, ethyl acetate in hexanes)

Методика

Methyl 6-chloro-5-nitronicotinate (1.1 g, 5.10 mmol) was added to ethyl thiomorpholine-3-carboxylate (2.0 g, 11.41 mmol) neat while stirring at room temperature. The viscous yellow reaction was heated to 90° C. for one hour and then allowed to cool back to room temperature. The reaction was diluted with dichloromethane (20 mL) and purified via column chromatography (220 g SiO2, 20-30% gradient, ethyl acetate in hexanes) to yield the title compound (1.71 g, 95%) as a yellow oil. [M+H] calc'd for C15H18N2O6S, 356; found, 356.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08822470B2uspto-grants-2014_09