[CH3:1][N:2]([CH3:15])[C:3]1([C:13]#N)[CH2:12][CH2:11][C:6]2([O:10][CH2:9][CH2:8][O:7]2)[CH2:5][CH2:4]1.[CH2:16]([Mg][Cl:21])[CH2:17][CH2:18]C.[Cl-].[NH4+].Cl[Si](C)(C)C>C1COCC1.CCOCC.O>[ClH:21].[CH2:13]([C:3]1([N:2]([CH3:15])[CH3:1])[CH2:12][CH2:11][C:6]2([O:10][CH2:9][CH2:8][O:7]2)[CH2:5][CH2:4]1)[CH2:16][CH2:17][CH3:18]
8-Dimethylamino-1,4-dioxa-spiro[4.5]decane-8-carbonitrile B-1 (10.5 g, 50 mmol) was placed in THF (150 ml), under argon and while cooling with ice. In the course of 15 min., 2M butyl-magnesium chloride in THF (62.5 ml, 125 mmol) was added dropwise, and the mixture was stirred for 16 h at room temperature. 20% ammonium chloride solution (37 ml) and water (50 ml) were added to the mixture, while cooling with ice, and extraction with ether (3×50 ml) was carried out. The organic phase was washed with water (1×50 ml) and saturated sodium chloride solution (1×50 ml), and the organic phase was dried with Na2SO4 and concentrated in vacuo. The crude product (2.05 g) was dissolved in ethyl methyl ketone (75 ml); ClSiMe3 (9.5 ml, 75 mmol) was added, while cooling with ice, and stirring was carried out for 6 h at room temperature. The resulting white precipitate was filtered out with suction and dried in vacuo.
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