反应详情

2-[4-(6-Chloro-benzo[b]thiophene-2-sulfonyl)-2-oxo-piperazin-1-ylmethyl]-6,7-dihydro-5H-benzothiazol-4-one (60 mg, 0.12 mmol) is dissolved in CHCl3 (4 mL) and sulfuric acid (0.5 mL) is added with vigorous stirring. Sodium azide (25 mg 0.4 mmol) is added and the reaction is stirred 1¾ h. The reaction is then added dropwise to a rapidly stirring mixture of K2CO3/H20/CH2Cl2. The organic phase is separated and washed with water, dried (MgSO4) and concentrated. The residue is purified by column chromatography (silica, 2% to 6% MeOH/CH2Cl2) to provide a mixture of two products.

1. additionThe reaction is then added dropwise to
2. stirringa rapidly stirring
3. customThe organic phase is separated
4. washwashed with water
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customThe residue is purified by column chromatography (silica, 2% to 6% MeOH/CH2Cl2)
8. customto provide
9. additiona mixture of two products