반응 #87631

ord-c521480019fd45eb94312a773d2c8503

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After completion of the reaction
  2. 2
    기타the reaction mass was quenched in ice water
  3. 3
    workup.STIRRINGstirred for 15 minutes
  4. 4
    여과The obtained solid product was filtered
  5. 5
    기타dried

실험 절차

To a solution of 2,6-dimethyl benzoic acid (6.8 g, 0.045 mmol) in conc. H2SO4 (100 mL), 2,2,2-trifluoro-N-(hydroxymethyl)acetamide (7.1 g, 0.049 mmol) was added and the reaction mixture was stirred at RT for 24 h. After completion of the reaction, the reaction mass was quenched in ice water and stirred for 15 minutes. The obtained solid product was filtered and dried to afford 7.0 g of the desired title product. 1H NMR (300 MHz, DMSO d6): δ 2.26 (s, 6H), 4.36 (t, J=12.3 Hz, 2H), 7.09 (m, 1H), 7.15 (m, 1H), 9.89-9.94 (m, 1H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09439890B2uspto-grants-2016_09