반응 #10388

반응 방정식

4-[3-(tert-Butoxycarbonylamino)-pyrrolidin-1-yl]-2,5-difluorobenzoic acid ethyl ester

isopropylamine

→

title compound

수율 28.1%

4-[3-(tert-Butoxycarbonylamino)pyrrolidin-1-yl]-5-fluoro-2-isopropylaminobenzoic acid ethyl ester

수율 28.1%

용매

dimethyl sulfoxide

반응 조건

후처리

1. 1
   기타The excess amine is removed
2. 2
   여과The residue is filtered
3. 3
   농축concentrated under vacuum to a thick oil
4. 4
   기타Purification by column chromatography (1:1:7 ethyl acetate/chloroform/hexanes)

실험 절차

4-[3-(tert-Butoxycarbonylamino)-pyrrolidin-1-yl]-2,5-difluorobenzoic acid ethyl ester (Example 2j, 5.4 g, 13.9 mmol), isopropylamine (40 mL, 469 mmol), and dimethyl sulfoxide (25 mL) are heated at 100° C. for 4 days in a sealed glass tube. The excess amine is removed by blowing in compressed air. The residue is filtered and concentrated under vacuum to a thick oil. Purification by column chromatography (1:1:7 ethyl acetate/chloroform/hexanes) to provide the title compound as a solid (1.6 g). MS: m/z 410 (MH+).

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