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Dimethylcarbamoyl Chloride → Isouron

HRID 2052201
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HRID 2052201 반응식
[CH3:1][N:2]([CH3:6])[C:3](Cl)=[O:4].[Cl-].[Al+3].[Cl-].[Cl-].[NH2:11][C:12]1[CH:16]=[C:15]([C:17]([CH3:20])([CH3:19])[CH3:18])[O:14][N:13]=1>C1(C)C=CC=CC=1.O>[CH3:1][N:2]([CH3:6])[C:3]([NH:11][C:12]1[CH:16]=[C:15]([C:17]([CH3:20])([CH3:19])[CH3:18])[O:14][N:13]=1)=[O:4]
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참가 물질

6

반응물 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 1714733-Isoxazolamine, 5-(1,1-dimethylethyl)-HCID 6451240Aluminum(III) Chloride

생성물 1

HCID 41648Isouron수율 99%

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매2회

실험 절차

N,N-Dimethylcarbamoyl chloride (7.91 g) and aluminum chloride (9.80 g) are added to toluene (100 ml), and the mixture is stirred at room temperature for 30 minutes. To this mixture is added 3-amino-5-t-butylisoxazole (9.81 g), and the resulting mixture is refluxed for 6 hours with stirring. After cooling, the reaction mixture is mixed with water, stirred at room temperature and shaken with toluene. The organic layer is evaporated to remove the toluene, whereby 1,1-dimethyl-3-(5-t-butyl-3-isoxazolyl)urea (14.63 g) is obtained. Yield is 98.9%. Melting point of the colorless crystalline product is 119 to 120.5° C. (after recrystallization from benzene).

후처리

  1. temperaturethe resulting mixture is refluxed for 6 hours
  2. stirringwith stirring
  3. temperatureAfter cooling
  4. stirringstirred at room temperature
  5. customThe organic layer is evaporated
  6. customto remove the toluene

출처 및 근거

ORD 기록
ord-bd124d54c5264ac58dc8a6d7b200d2b8
출처 데이터셋
uspto-grants-1980_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04183856

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