반응 #11751

반응 방정식

(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-acetic acid

sulfamide

→

title compound

수율 12.7%

N-[(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-acetyl]-sulfamide

수율 12.7%

용매

thionyl chloride

반응 조건

후처리

1. 1
   농축The reaction was concentrated to dryness
2. 2
   workup.DISSOLUTIONthe crude acid chloride was dissolved in 1,4-dioxane (4 mL)
3. 3
   농축The reaction was concentrated
4. 4
   기타chromatographed on silica gel

실험 절차

A solution of (5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-acetic acid (0.10 g, 0.21 mmol) in thionyl chloride (2 mL) was stirred at ambient temperature for two hours. The reaction was concentrated to dryness and the crude acid chloride was dissolved in 1,4-dioxane (4 mL) followed by addition of sulfamide (0.022 g, 0.23 mmol). The reaction was stirred at ambient temperature for 3 days. The reaction was concentrated and chromatographed on silica gel to give the title compound (0.014 g, LRMS: 525.1).

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