FC(F)(F)C(O)=O.ClCCl.[CH3:11][O:12][C:13](=[CH2:16])[C:14]#[N:15].[CH2:17]([N:24]([CH2:30]OC)[CH2:25][Si](C)(C)C)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(=O)([O-])O.[Na+]>C(N(CC)CC)C>[CH2:17]([N:24]1[CH2:25][CH2:16][C:13]([C:14]#[N:15])([O:12][CH3:11])[CH2:30]1)[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1To a mixture of 1.2 g trifluoroacetic acid and 1.2 g triethylamine in 200 ml dry dichloromethane 8.3 g (90 mmol, 90% proof) 2-methoxyacrylonitrile (J. Chem. Soc. 520, 1942) are added. Thereafter 28.5 g N-benzyl-N-methoxymethyl-N-(trimethylsilylmethyl)amine (Chem. Letters 1117, 1984) are added, and the mixture is stirred overnight at room temperature. The mixture is treated with a saturated solution of sodium hydrogencarbonate, dried with magnesium sulfate, and finally the organic solvents are removed in vacuo and the residue is distilled.
Wird geladen…
