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Ethanol → Imidazole,2-nitro-1-(3-methoxy-2-fluoro)propyl-

HRID 1464422
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인쇄 미리보기

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HRID 1464422 반응식
O[CH:2]([CH2:12][O:13][CH3:14])[CH2:3][N:4]1[CH:8]=[CH:7][N:6]=[C:5]1[N+:9]([O-:11])=[O:10].CCN(S(F)(F)[F:21])CC.C(O)C>O1CCOCC1>[F:21][CH:2]([CH2:12][O:13][CH3:14])[CH2:3][N:4]1[CH:8]=[CH:7][N:6]=[C:5]1[N+:9]([O-:11])=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 26105MisonidazoleHCID 123472(Diethylamino)sulfur trifluoride2회

생성물 1

HCID 14458239Imidazole,2-nitro-1-(3-methoxy-2-fluoro)propyl-수율 52%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of 914 mg (4.54 mmol) of 1-(2'-hydroxy-3'-methoxypropyl)-2-nitroimidazole in 5.0 ml of dry dioxane, 1.00 g (6.20 mmol) of DAST was dropwise added with cooling by ice and then reacted for 2 hours at room temperature with stirring. After reaction, to the solution, 5.0 ml of ethanol was added to decompose excess DAST. The solution was then concentrated and subjected to isolation and purification by silica gel column chromatography to give 480 mg of 1-(2-'-fluoro-3'-methoxypropyl)-2-nitroimidazole.

후처리

  1. temperaturewith cooling by ice
  2. customreacted for 2 hours at room temperature
  3. customAfter reaction
  4. concentrationThe solution was then concentrated
  5. customsubjected to isolation and purification by silica gel column chromatography

출처 및 근거

ORD 기록
ord-2adec24f4e3b40cc9faa6cf0182a4ecc
출처 데이터셋
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05304654

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