N,N-Dimethyl-O-(methylsulfonyl)hydroxylamine → HCID 178506778, 화합물
반응식
[CH:1]1([Li:6])[CH:5]=[CH:4][CH:3]=[CH:2]1.[N:7](OS(C)(=O)=O)([CH3:9])[CH3:8].C([Li])CCC>C1COCC1.CCCCCC>[CH3:8][N:7]([C:1]1([Li:6])[CH:5]=[CH:4][CH:3]=[CH:2]1)[CH3:9][CH:1]1([Li:6])[CH:5]=[CH:4][CH:3]=[CH:2]1.[N:7](OS(C)(=O)=O)([CH3:9])[CH3:8].C([Li])CCC>C1COCC1.CCCCCC>[CH3:8][N:7]([C:1]1([Li:6])[CH:5]=[CH:4][CH:3]=[CH:2]1)[CH3:9]A solution of 3 g of cyclopentadienyllithium (0.042 moles) in 30 ml of THF was added slowly at −30° C. to a solution of 5.9 g of compound 6 (0.042 moles) in 20 ml of THF. The mixture was then heated to −20° C. and stirred for 30 min. Hexane was then added and the solution was filtered. 1.8 ml of a 2.3 molar solution of butyllithium (0.042 moles) in hexane were then added at −20° C. to produce a precipitate. The precipitate was filtered off and washed with twice 20 ml of hexane. After drying under vacuum, 2.0 g (40% of the theoretical yield) of compound 7 were obtained in the form of a white powder; cf. Angew. Chem., Int. Ed. Engl. 19, (1980), 1010. 1H NMR (400 MHz, THF): δ=5.34 (bd, J=2.2 Hz, 2H); 5.15 (bd, J 2.2 Hz, 2H); 2.56 (s, 6H).
불러오는 중…
