Sulfuric Acid → HCID 22279875, compound

Participants

Reaction Steps

2-Amino-2-methyl-4-[4-(5-phenylpent-1-ynyl)thiophen-2-yl]butan-1-ol hydrochloride (178 mg, 0.49 mmol) obtained in Example 26 (i) was dissolved in methanol (2 ml), and 6N sulfuric acid (2 ml) was added thereto followed by heating under reflux for 4 hours. After the reaction solution was made alkaline with a 1N aqueous sodium hydroxide solution, the resulting solution was extracted with dichloromethane. The dichloromethane layer was dried over anhydrous sodium sulfate, and the solvent was evaporated in vacuo. The residue was dissolved in 1,4-dioxane (2 ml), and the dioxane solution of 4N hydrochloric acid was added thereto in an ice bath, and then the solvent was evaporated under reduced pressure. The obtained white solid was washed with ether, and dried to give the title compound (100 mg, 53% yield).

Provenance & Evidence