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Triethylamine → (2E)-3-(4-Fluoro-2-methoxyphenyl)-2-propenoyl azide

HRID 1852113
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HRID 1852113 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[C:10](O)=[O:11])=[C:4]([O:13][CH3:14])[CH:3]=1.C1(P([N:29]=[N+:30]=[N-:31])(C2C=CC=CC=2)=O)C=CC=CC=1.CCN(CC)CC>C1C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[C:10]([N:29]=[N+:30]=[N-:31])=[O:11])=[C:4]([O:13][CH3:14])[CH:3]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 23150778(2E)-3-(4-Fluoro-2-methoxyphenyl)-2-propenoic acid

생성물 1

HCID 86683195(2E)-3-(4-Fluoro-2-methoxyphenyl)-2-propenoyl azide수율 76.5%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

(E)-3-(4-fluoro-2-methoxyphenyl)acrylic acid (1.22 g, 6.22 mmol), diphenylphosphinyl azide (1.273 mL, 5.91 mmol), and Et3N (1.734 mL, 12.44 mmol) were dissolved in benzene and stirred for 16 h. The solution was concentrated under vacuum and the residue was purified by silica gel chromatography using 20% EtOAc/Hexanes to give (E)-3-(4-fluoro-2-methoxyphenyl)acryloyl azide (1.0 g, 73% yield).

후처리

  1. concentrationThe solution was concentrated under vacuum
  2. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-d2d1140c6ef54b398004eff84696f3c1
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08957203B2

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