Реакция #44157

ord-e43dbf51330b477594329fda39fed113

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Промывкаwashed with water (50 mL), aqueous hydrochloric acid (1N, 2×50 mL)
  2. 2
    СушкаThe organic layer was dried over sodium sulfate
  3. 3
    Концентрированиеconcentrated under reduced pressure
  4. 4
    ДругоеThe crude was purified by flash chromatography on silica gel
  5. 5
    Промывкаeluting with ethyl acetate-cyclohexane (50:50)

Методика

Methanesulfonyl chloride (0.124 mL) was added dropwise to a stirred solution of 1-[3-(2-hydroxyethyl)phenyl]-2-pyrrolidinone (0.30 g) and triethylamine (0.42 mL) in dichloromethane (10 mL) at room temperature under an inert atmosphere. The solution was stirred for 2 hours. The reaction mixture was diluted with ethyl acetate (50 mL) and washed with water (50 mL), aqueous hydrochloric acid (1N, 2×50 mL), a saturated aqueous solution of sodium hydrogencarbonate (50 mL) and brine (50 mL). The organic layer was dried over sodium sulfate and concentrated under reduced pressure. The crude was purified by flash chromatography on silica gel, eluting with ethyl acetate-cyclohexane (50:50) to afford the title compound in 93% yield (0.384 g).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07732600B2uspto-grants-2010_06