Triethylsilane → HCID 17848741, compound

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Reaction Steps

Triethyl silane (22.2 ml, 139 mmol) was added under a nitrogen atmosphere to a solution of 1-(1-acetyl-2,3,4,5-tetrahydro-1H-1-benzazepin-8-yl)-3-(dimethylamino)-1-propanone (5.00 g, 17.3 mmol) obtained in Reference Example 8 in trifluoroacetic acid, and then the mixture was stirred at room temperature for 5 days. After the solvent was distilled away under reduced pressure, ether was added to the residues which were then extracted with water. The aqueous layer was made basic with 8 N aqueous sodium hydroxide and then extracted with ethyl acetate. The extract was washed with a saturated saline solution and dried over anhydrous sodium sulfate, and the solvent was distilled away under reduced pressure. The resultant residues were purified by alumina column chromatography (developing solvent; hexane:ethyl acetate=1:1), whereby the title compound (2.74 g) was obtained as oily matter.

Provenance & Evidence