反応 #87631

反応方程式

2,6-dimethyl benzoic acid

2,2,2-trifluoro-N-(hydroxymethyl)acetamide

→

desired title product

3-((2,2,2-trifluoroacetamido)methyl)-2,6-dimethylbenzoic acid

溶媒

H2SO4

反応条件

後処理

1. 1
   その他After completion of the reaction
2. 2
   その他the reaction mass was quenched in ice water
3. 3
   workup.STIRRINGstirred for 15 minutes
4. 4
   ろ過The obtained solid product was filtered
5. 5
   その他dried

実験手順

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).

出典