反应详情

To a saturated solution of HCl(g) in dioxane (100 mL) was added 7-(2-{[2-(4-cyanophenoxy)ethyl]methanesulfonylamino}ethyl)-9-oxa-3,7-diaza-bicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester (3.5 g, 0.0070 mol; see step (i) above), after which the reaction was stirred for 1 h. On completion of the reaction (as determined by TLC), dioxane was decanted and product (semi-solid) dissolved in methanol (25 mL). After concentrating the methanol, dry ether (50 mL) was added and the solvent was again concentrated. This was repeated twice and finally the product was dried under high vacuum. Yield: 3.0 g (99%).

1. customwas decanted
2. dissolutionproduct (semi-solid) dissolved in methanol (25 mL)
3. concentrationAfter concentrating the methanol, dry ether (50 mL)
4. additionwas added
5. concentrationthe solvent was again concentrated
6. customfinally the product was dried under high vacuum