反应详情

5 g cis(+)-2,3-dihydro-3-hydroxy-2-(4-methoxyphenyl)-1,5-benzothiazepin-4(5H)-one, 2.9 g 2-methyl-3-dimethylaminopropylchloride hydrochloride, 5.7 g K2CO3, 1.4 ml H2O were reacted in 75 ml acetone, according to the procedure as in Example 1 (a), then reacted with 70 ml acetic anhydride, (see Example 1 (b)). The crude was treated with ethyl ether and the so obtained solid is filtered off and the solution was evaporated to dryness. This procedure was repeated. 4.3 g residue were dissolved in isopropyl alcohol and treated with 1.2 g oxalic acid. A solid, which was crystallized from acetone-ethyl ether, was obtained; m.p. 84°-89° C.; [α]D20 =119.3 (H2O).

1. filtrationthe so obtained solid is filtered off
2. customthe solution was evaporated to dryness
3. dissolution4.3 g residue were dissolved in isopropyl alcohol
4. additiontreated with 1.2 g oxalic acid
5. customA solid, which was crystallized from acetone-ethyl ether
6. customwas obtained