Water → HCID 54241509, compound

Participants

Reaction Steps

To a solution of 11.2 g of the above amine in 50 ml of pyridine is added 6.35 g of 1,3,6-naphthalenetrisulfonyl chloride. The resulting solution is heated on a steam bath for one hour, cooled to room temperature and poured into cold water with separation of an oil. The mixture is extracted with methylene chloride. The methylene chloride extract is washed with 0.5N hydrochloric acid, then with water and dried over magnesium sulfate. The solvent is removed and the resulting oil is dissolved in benzene:acetone (7:3) and passed through a bed of magnesol on a sintered glass funnel. The cake is washed with additional benzene:acetone (7:3). The filtrate and washings are combined and evaporated and dried in vacuo to yield 11.9 g of the product of the example as a cream colored solid.

Provenance & Evidence