反应详情

To a suspension of the title B compound in Example 9, 2-(2,4-dimethoxy-benzyl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one, (13.87 g, 48.4 mmol) and 4-bromomethylbenzoic acid (10.42 g, 48.4 mmol) in CH2Cl2 (150 mL), DBU (14.5 mL, 96.9 mmol) is added at once and the mixture is stirred at RT overnight. The reaction mixture is washed with 1N aqueous HCl, and brine, dried over anhydrous MgSO4 and evaporated to a small volume to crystallize the product. The solid is collected by filtration, washed with ethyl ether and dried under high vacuum to afford 4-[5-(2,4-dimethoxy-benzyl)-1,1,4-trioxo-1,2,5-thiadiazolidin-2-ylmethyl]-benzoic acid: mp=175-177° C.; [M−1]−=419.

1. additionis added at once and the mixture
2. washThe reaction mixture is washed with 1N aqueous HCl, and brine
3. dry with materialdried over anhydrous MgSO4
4. customevaporated to a small volume
5. customto crystallize the product
6. filtrationThe solid is collected by filtration
7. washwashed with ethyl ether
8. customdried under high vacuum