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

HRID 28256
ノート
印刷プレビュー

反応式

HRID 28256 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
135 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ba867d69358d4678ae07e3c7210e9ee7
出典データセット
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04225723

反応ノート

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