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

HRID 1164367
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HRID 1164367 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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).

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후처리

  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

출처 및 근거

ORD 기록
ord-565c451729094ad8b8df8c8fdbfd1de6
출처 데이터셋
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04369186

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