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Water → HCID 70874980, 화합물

HRID 2172263
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HRID 2172263 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH2:21][C:22]([OH:35])([CH3:34])[CH2:23][CH2:24][N:25]3[CH:29]=[C:28]([N+:30]([O-:32])=[O:31])[N:27]=[C:26]3Cl)=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].O>CN(C)C=O>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH2:21][C:22]3([CH3:34])[O:35][C:26]4=[N:27][C:28]([N+:30]([O-:32])=[O:31])=[CH:29][N:25]4[CH2:24][CH2:23]3)=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24758Sodium hydrideHCID 70873547HCID 70873547, 화합물

생성물 1

HCID 70874980HCID 70874980, 화합물수율 53.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-{4-[4-(2-Chloro-4-nitroimidazol-1-yl)-2-hydroxy-2-methylbutoxy]phenyl}piperazine-1-carboxylic acid tert-butyl ester (2.12 g) was dissolved in dimethylformamide (21 ml). 60% sodium hydride (0.24 g) was added thereto, and the mixture was stirred at room temperature for 3 hours. Water was added to the reaction mixture, the mixture was subjected to extraction with methylene chloride, and then dried over sodium sulfate. After filtering, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (methylene chloride:ethyl acetate=1:0→methylene chloride:ethyl acetate=1:1) to afford the title compound as a colorless powder (1.05 g).

후처리

  1. extractionthe mixture was subjected to extraction with methylene chloride
  2. dry with materialdried over sodium sulfate
  3. filtrationAfter filtering
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (methylene chloride:ethyl acetate=1:0→methylene chloride:ethyl acetate=1:1)

출처 및 근거

ORD 기록
ord-9d1e0db7cec649769a40dee49cf15da9
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09051333B2

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