반응 #2396985

ord-f80843538a39415ab3a3c91b0a471b15

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGAfter an additional six hours of stirring the mixture
  2. 2
    추출was extracted with saturated sodium bicarbonate (3×100 mL)
  3. 3
    건조The organic layer was dried over sodium sulfate
  4. 4
    농축concentrated to a total volume of 75 mL

실험 절차

To a suspension of n-chloroperbenzoic acid (14.5 g) in dry methylene chloride (150 mL) was added a solution of 2-benzyl-4-(4-pyridyl)thiazole (15.1 g, 0.06 mol) in methylene chloride (125 mL) over thirty minutes. The mixture was allowed to stir overnight at room temperature then an additional portion of m-chloroperbenzoic acid (3.00 g) was added. After an additional six hours of stirring the mixture was extracted with saturated sodium bicarbonate (3×100 mL). The organic layer was dried over sodium sulfate, and concentrated to a total volume of 75 mL. Dilution with ether (200 mL) afforded 4-[2-(phenylmethyl)-4-thiazolyl]pyridine -1-oxide (15.3 g, 95%). Recrystallization from ethanol/ether afforded an analytical sample. mp. 170°-172° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04697012uspto-grants-1987_09