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1,4-Dioxane → 4,5-dichloroimidazole-2-carboxylic acid N-(2-cyanoethyl)-N-methylamide

HRID 1164367
ノート
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反応式

HRID 1164367 の反応式
Cl.[CH3:2][NH:3][CH2:4][CH2:5][C:6]#[N:7].[Cl:8][C:9]1[C:13]([Cl:14])=[N:12][C:11](=[C:15](Cl)Cl)[N:10]=1.[O:18]1CCOCC1>>[C:6]([CH2:5][CH2:4][N:3]([CH3:2])[C:15]([C:11]1[NH:12][C:13]([Cl:14])=[C:9]([Cl:8])[N:10]=1)=[O:18])#[N:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 312751,4-DioxaneHCID 124825724,5-Dichloro-2-(dichloromethylidene)-2H-imidazoleHCID 205119223-Methylaminopropionitrile hydrochloride

生成物 1

HCID 539822874,5-dichloroimidazole-2-carboxylic acid N-(2-cyanoethyl)-N-methylamide収率 67%

実験手順

24 g (0.2 mol) of 3-methylaminopropionitrile hydrochloride were added to a solution of 21.8 g (0.1 mol) of 4,5-dichloro-2-dichloromethylene-imidazole in 100 ml of dioxane and the mixture was heated to the reflux temperature for two hours, while stirring. After cooling, the product was precipitated with water, filtered off, washed with water and dried. In this way, 16.5 g (67% of theory) of 4,5-dichloroimidazole-2-carboxylic acid N-(2-cyanoethyl)-N-methylamide were obtained. Melting point: 184° C. (from acetonitrile).

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturethe mixture was heated to the reflux temperature for two hours
  2. temperatureAfter cooling
  3. customthe product was precipitated with water
  4. filtrationfiltered off
  5. washwashed with water
  6. customdried

出典と根拠

ORDレコード
ord-565c451729094ad8b8df8c8fdbfd1de6
出典データセット
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04369186

反応ノート

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