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- W2076201558 abstract "C22H20N4O8S, triclinic, P1 (no. 2), a =8 .408(6) A, b =9 .842(7) A, c =1 5.15(1) A, * =1 08.369(8)°, ) =1 01.227(9)°, ’ =9 6.479(8)°, V =1 146.8 A 3 , Z =2 , Rgt(F) =0 .042, wRref(F 2 ) =0 .130, T =2 96 K. Source of material Protocatechuic acid (5.0 g, 0.0333 mol) wa sa dded to 15 mL acetic anhydride, and allowed to react at 140 °C for 4h ,t hen concentrated. From the crude product, the white powder of acetyl protocatechuic acid was obtained by recrystallization from ethanol. To the acetyl protocatechuic acid (5.0 g, 0.0210 mol), SOCl2 (15 mL) was adde da nd allowed to react for 5hu nder reflux .T he excess of SOCl2 wa se vaporate du nder vacuum and th ec rude produc tw as used fo rt he amidatio ns tep. Am ixture of sulfamonomethoxine (5.9 g, 0.0210 mol) in 30 mL of THF and 5m Lp yridine was added to acetyl protocatechuic chloride and allowed to react for 2h ours in an ice-bath and then kept at room temperature for about 24 hours. When the reaction was complete, the solvent was evaporated under vacuum ,a nd the residue was washed with wate ra nd recrystallized from MeOH and THF to afford th et itle compound. Experimental details All Ha toms were positioned geometrically with d(C—H) =0 .930.96 Aa nd refined as riding with Uiso =1 .2 Ueq." @default.
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- W2076201558 date "2012-01-01" @default.
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- W2076201558 title "Crystal structure of 3,4-bis(acetyloxy)-N-{4-[(6-methoxy-4- pyrimidinyl)aminosulfonyl]phenyl}benzamide, C22H20N4O8S" @default.
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- W2076201558 doi "https://doi.org/10.1524/ncrs.2012.0060" @default.
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