反应详情

To a mixture of paracetamol (150 g, 992 mmol), anhydrous K2CO3 (540 kg, 3.91 mol) and sodium iodide (18 gm, 120 mmol) in anhydrous acetone (3 L) was added methyl 2-chloropropionate (180 g, 1.469 mmol) and refluxed for 80 hours. The acetone was distilled off and water (3 L) was added. Crude 8 was extracted into chloroform, dried over Na2SO4, distilled and hexane (750 ml) was added. The solids were then filtered and recrystallised in methanol to give pure 8 (95 g, 40.4%) as a white powder with an m.p between 96.5-98.2° C.

1. temperaturerefluxed for 80 hours
2. distillationThe acetone was distilled off
3. additionwater (3 L) was added
4. extractionCrude 8 was extracted into chloroform
5. dry with materialdried over Na2SO4
6. distillationdistilled
7. additionhexane (750 ml) was added
8. filtrationThe solids were then filtered
9. customrecrystallised in methanol