反应 #1323088
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07291619B2
反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a 50 mL flask containing 2-flourobenzene sulfonamide (200 mg, 1.14 mmol, 1 eq.) and piperazine (245 mg, 2.84 mmol, 2.5 eq) was added 20 mL of dioxane. The solution was heated to 100° C. for about 4 hours. More piperazine (200 mg, 2.32 mmol, 2 eq.) was added and the solution was heated to 100° C. for another 72 hours. The solution was concentrated to an oil and dissolved in 30 mL of 0.1 M pH 7.0 phosphate buffer. The aqueous solution was extracted with CH2Cl2 (3×30 mL). The combined organic extracts were dried over Na2SO4 and concentrated to yield about 275 mg (1.14 mmol, 100%) of the title compound. LRMS (ESI+): 242.1 (M+H). the solution was heated to 100° C. for another 72 hours The solution was concentrated to an oil dissolved in 30 mL of 0.1 M pH 7.0 phosphate buffer The aqueous solution was extracted with CH2Cl2 (3×30 mL) The combined organic extracts were dried over Na2SO4 concentrated
来源 ID: ord-c6635f7be9364a228c7cd1679de03ec1