反应详情

5.5 mL water, 20 mL MeCN, 0.36 g KBr, 4-MeOTEMPO (0.15 g), and 10 g of 2,2,3-trifluoro-3-(1,1,2,2,3,3-hexafluoro-3-trifluoromethoxy-propoxy)-propan-1-ol are placed in a 50 ml glass flask equipped with a dropping funnel and stirrer. 36 mL of a 15% wt. aq. NaOCl solution buffered to pH 8-9 were added via the dropping funnel in 3 portions over two days while stirring at room temperature. Concentrated sulphuric acid and water were added to make the reaction mixture acidic (pH 1 to 2). The reaction mixture was extracted three times with diethyl ether. The combined ether phases were dried over magnesium sulphate and the solvent was removed by a rotary evaporator. The residue was distilled to give 8.4 g of the acid (b.p. 58 C, 1.6 mmHg). Yield: 81%.

1. customequipped with a dropping funnel and stirrer
2. additionwere added via the dropping funnel in 3 portions over two days
3. extractionThe reaction mixture was extracted three times with diethyl ether
4. dry with materialThe combined ether phases were dried over magnesium sulphate
5. customthe solvent was removed by a rotary evaporator
6. distillationThe residue was distilled