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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 54389470, 화합물 → HCID 54245016, 화합물

HRID 356577
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HRID 356577 반응식
[C:1]([O:5][C:6]([NH:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[CH:15][C:16]([N+:23]([O-:25])=[O:24])=[C:17]([CH:19]([OH:22])[CH:20]=[CH2:21])[CH:18]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(Cl)(Cl)Cl.[O-2].[O-2].[Mn+4]>[C:1]([O:5][C:6]([NH:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:14]=[CH:15][C:16]([N+:23]([O-:25])=[O:24])=[C:17]([C:19](=[O:22])[CH:20]=[CH2:21])[CH:18]=1)=[O:7])([CH3:2])([CH3:3])[CH3:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 54389470HCID 54389470, 화합물

생성물 1

HCID 54245016HCID 54245016, 화합물수율 63%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 6212Chloroform용매

반응 조건

온도
50 °C

실험 절차

1-(5'-(3"-t-Butoxycarbonylaminopropyloxy)-2'-nitrophenyl)-2-propen-1-ol (9.66 g) is dissolved in chloroform (300 ml), and thereto is added active manganese dioxide (72 g), and the mixture is refluxed. After the reaction is completed, the inorganic materials are removed by filtration through a pad of Celite, and the filtrate is concentrated, stirred at 50° C. for 6 hours, and thereto is added ethyl acetate. The mixture is washed with a saturated sodium chloride solution, and dried over sodium sulfate. The residue is purified by silica gel column chromatography to give 1-[5'-(3"-t-butoxycarbonylaminopropyloxy)-2'-nitrophenyl]-2-propen-1-one (6.01 g) as a yellow product.

후처리

  1. temperaturethe mixture is refluxed
  2. customthe inorganic materials are removed by filtration through a pad of Celite
  3. concentrationthe filtrate is concentrated
  4. additionis added ethyl acetate
  5. washThe mixture is washed with a saturated sodium chloride solution
  6. dry with materialdried over sodium sulfate
  7. customThe residue is purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-dcbe8a0d0be649899d877a0d7b07af4e
출처 데이터셋
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05837673

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