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Tetrahydrofuran → HCID 19825152, 화합물

HRID 727822
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HRID 727822 반응식
CN(C)S([N:6]1[CH:10]=[C:9](C2C=CC=CC=2)[N:8]=[C:7]1[CH:17]=[N:18]O)(=O)=O.[H-].[Na+].Cl[C:24]([O:26][CH2:27][CH3:28])=[O:25].C(O[CH2:33][CH3:34])(=O)C.O1[CH2:39][CH2:38][CH2:37][CH2:36]1>>[C:17]([CH:7]1[N:6]([C:34]2[CH:33]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH:10]=[CH:9][N:8]1[C:24]([O:26][CH2:27][CH3:28])=[O:25])#[N:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 8028Tetrahydrofuran2회HCID 8857Ethyl AcetateHCID 10928Ethyl chloroformateHCID 24758Sodium hydrideHCID 136341188HCID 136341188, 화합물

생성물 1

HCID 19825152HCID 19825152, 화합물

실험 절차

1-(dimethylsulphamoyl)-2-(hydroxyiminomethyl)-4-phenylimidazole, m.p 165°-170° (dec.). A slurry of this product (0.882 g) in dry tetrahydrofuran (20 ml) was added to sodium hydride (90 mg of 80g suspension in oil) in dry tetrahydrofuran. After 1.5 hours at room temperature ethyl chloroformate (0.285 ml) was added and the mixture stirred overnight. The mixture was then added to ethyl acetate and worked up in conventional manner to give a viscous oil. This was purified by flash column chromatography to give 2-cyano-1-ethoxycarbonyl-3-phenylimidazole, m.p. 109°-111°. (Compound 3)

후처리

  1. customto give a viscous oil
  2. customThis was purified by flash column chromatography

출처 및 근거

ORD 기록
ord-e4378b2e678043359ee6a5272d3a1ed0
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05045557

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