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Imidazole → 1-[2-Cyano-2-(2,4-dichlorophenyl)hexyl]imidazole hydrochloride

HRID 28256
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HRID 28256 반응식
CS(O[CH2:6][C:7]([C:20]#[N:21])([C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=1[Cl:19])[CH2:8][CH2:9][CH2:10][CH3:11])(=O)=O.[NH:22]1[CH:26]=[CH:25][N:24]=[CH:23]1.CN(C)C=O>O>[ClH:18].[C:20]([C:7]([C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=1[Cl:19])([CH2:8][CH2:9][CH2:10][CH3:11])[CH2:6][N:22]1[CH:26]=[CH:25][N:24]=[CH:23]1)#[N:21]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 795ImidazoleHCID 6228DimethylformamideHCID 233399252-Cyano-2-(2,4-dichlorophenyl)hexyl methane sulfonate

생성물 1

HCID 233399171-[2-Cyano-2-(2,4-dichlorophenyl)hexyl]imidazole hydrochloride수율 68%

시약·촉매·용매 1

HCID 962Water용매

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온도
135 °C

실험 절차

A mixture of 2-cyano-2-(2,4-dichlorophenyl)hexyl methane sulfonate (100 g., 0.29 mole), imidazole (100 g., 1.5 mole) and N,N-dimethylformamide (5 ml.) is heated with stirring at 135° C. overnight. The reaction mixture is poured into water and extracted with ether. The combined ether extracts are dried over magnesium sulfate. The drying agent is filtered and into the ethereal solution is bubbled dry hydrogen chloride gas. The white solid which precipitates is collected and dried to give 70.4 g. (68%) of the expected product, which is identified by nmr.

후처리

  1. temperatureis heated
  2. extractionextracted with ether
  3. dry with materialThe combined ether extracts are dried over magnesium sulfate
  4. filtrationThe drying agent is filtered and into the ethereal solution
  5. customis bubbled dry hydrogen chloride gas
  6. customThe white solid which precipitates
  7. customis collected
  8. customdried
  9. customto give 70.4 g

출처 및 근거

ORD 기록
ord-ba867d69358d4678ae07e3c7210e9ee7
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04225723

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