反应详情

A suspension composed of 290 mg (1.21 mmol) of 2,3,3a,4-tetrahydro-1H-pyrrolo[2,1-c][1,2,4]benzothiadiazin-7-ol 5,5-dioxide, 465 mg (1.82 mmol) of the compound obtained in Step D, 330 mg (1.82 mmol) of copper(II) acetate, 294 μl (3.64 mmol) of pyridine and about 3.5 g of 4 Å molecular sieve in 35 ml of CH2Cl2 is stirred for 5 hours at ambient temperature. The reaction mixture is filtered and rinsed with CH2Cl2/MeOH (1/1). The filtrate is concentrated and then directly applied to a silica column, eluting with a mixture of CH2Cl2/acetone 96/4. The fractions containing the expected compound are collected and evaporated and the residue is taken up in a small amount of ethyl ether. After filtering off the solid, the title compound is collected in the form of a white powder.

1. filtrationThe reaction mixture is filtered
2. washrinsed with CH2Cl2/MeOH (1/1)
3. concentrationThe filtrate is concentrated
4. washeluting with a mixture of CH2Cl2/acetone 96/4
5. additionThe fractions containing the expected compound
6. customare collected
7. customevaporated
8. filtrationAfter filtering off the solid
9. customthe title compound is collected in the form of a white powder