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Phosphorus oxychloride → HCID 66839224, 화합물

HRID 546756
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인쇄 미리보기

반응식

HRID 546756 반응식
[CH3:1][O:2][C:3]1[N:8]=[C:7](/[CH:9]=[CH:10]/[C:11]([NH2:13])=O)[CH:6]=[CH:5][C:4]=1[N:14]1[CH:18]=[C:17]([CH3:19])[N:16]=[CH:15]1.P(Cl)(Cl)(Cl)=O>>[CH3:1][O:2][C:3]1[N:8]=[C:7](/[CH:9]=[CH:10]/[C:11]#[N:13])[CH:6]=[CH:5][C:4]=1[N:14]1[CH:18]=[C:17]([CH3:19])[N:16]=[CH:15]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 66839442(E)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]acrylamide

생성물 1

HCID 66839224HCID 66839224, 화합물수율 68.9%

반응 조건

온도
90 °C

실험 절차

A mixture of (E)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]acrylamide (3.54 g) and phosphorus oxychloride (12 ml) was stirred at 90° C. for one hour. The reaction solution was concentrated under reduced pressure and then diluted with ice water, chloroform and aqueous ammonia, and the organic layer was separated. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was diluted with ether and the precipitated crystals were collected by filtration. The crystals were washed with ether and then air-dried to obtain 2.27 g of the title compound. The property value of the compound is as follows.

후처리

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additiondiluted with ice water, chloroform and aqueous ammonia
  3. customthe organic layer was separated
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionThe residue was diluted with ether
  7. filtrationthe precipitated crystals were collected by filtration
  8. washThe crystals were washed with ether
  9. customair-dried

출처 및 근거

ORD 기록
ord-34b11d30932d42f0a57346c0496b0ad3
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07935815B2

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