反応 #595335

ord-01901bcf48d84da2958c5005252af0f4

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A melt is formed
  2. 2
    workup.STIRRINGstirred at RT overnight
  3. 3
    その他The precipitate formed
  4. 4
    ろ過is filtered off
  5. 5
    その他dried at 40° C. in a vacuum
  6. 6
    その他drying cabinet overnight

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09095582B2uspto-grants-2015_08