反应详情

21.8 g (119 mmol) of N-Methoxy-N-methyl-2-trifluoromethyl-acrylamide (67) and 36.1 ml (29.6 mmol) of 2-(trimethylsiloxy)-1,3-butadiene were mixed and divided into 3 portions. Each portion was treated at 120° C. under microwave irradiation for 2 h. The combined reaction products were then diluted using 150 ml of THF, 100 ml of a 5% aqueous solution of HCl was added and stirred for 1 h at ambient temperature. Afterwards, the mixture was extracted three times using 200 ml of ethyl acetate each, dried using MgSOt and evaporated to yield 18.0 g, used without further purification. Rt=0.72 min (Method P).

1. additionEach portion was treated at 120° C. under microwave irradiation for 2 h
2. customThe combined reaction products
3. additionwere then diluted
4. additionwas added
5. extractionAfterwards, the mixture was extracted three times
6. customdried
7. customevaporated
8. customto yield 18.0 g
9. customused without further purification