반응식
[CH3:1][O:2][N:3]([CH3:12])[C:4](=[O:11])[C:5]([C:7]([F:10])([F:9])[F:8])=[CH2:6].C[Si](C)(C)[O:15][C:16]([CH:18]=[CH2:19])=[CH2:17].Cl>C1COCC1>[CH3:1][O:2][N:3]([CH3:12])[C:4]([C:5]1([C:7]([F:10])([F:8])[F:9])[CH2:19][CH2:18][C:16](=[O:15])[CH2:17][CH2:6]1)=[O:11]참가 물질
5
실험 절차
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).
후처리
- additionEach portion was treated at 120° C. under microwave irradiation for 2 h
- customThe combined reaction products
- additionwere then diluted
- additionwas added
- extractionAfterwards, the mixture was extracted three times
- customdried
- customevaporated
- customto yield 18.0 g
- customused without further purification
출처 및 근거
- ORD 기록
- ord-c3c6b04c9592419b8801d03943793262
- 출처 데이터셋
- uspto-grants-2013_03
- 특허 번호
- US08399482B2
연결된 노트
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