반응 #595335

ord-01901bcf48d84da2958c5005252af0f4

반응 방정식

Cc1cc(C(N)=O)ccc1F
4-fluoro-3-methylbenzamide
O=C(CCl)CCl
1,3-dichloro-acetone
O=S(=O)(O)O
sulfuric acid
Cc1cc(-c2nc(CCl)co2)ccc1F
4-(Chloromethyl)-2-(4-fluoro-3-methylphenyl)-1,3-oxazole

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A melt is formed
  2. 2
    workup.STIRRINGstirred at RT overnight
  3. 3
    기타The precipitate formed
  4. 4
    여과is filtered off
  5. 5
    기타dried at 40° C. in a vacuum
  6. 6
    기타drying cabinet overnight

실험 절차

2.00 g (12.80 mmol) of 4-fluoro-3-methylbenzamide and 1.79 g (14.08 mmol) of 1,3-dichloro-acetone are stirred at 130° C. for 2 days. A melt is formed. The mixture is then cooled to RT, 3.0 ml of conc. sulfuric acid are added carefully at this temperature and the mixture is stirred for 15 min. The resulting suspension is poured into 20 ml of ice-water and stirred at RT overnight. The precipitate formed is filtered off and dried at 40° C. in a vacuum drying cabinet overnight.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09095582B2uspto-grants-2015_08