Dimethylcarbamoyl Chloride → HCID 13228710, 화합물

HRID 615812노트

반응식

HRID 615812 반응식
[NH2:1][C:2]1[CH:6]=[C:5]([C:7]([CH3:10])([CH3:9])[CH3:8])[NH:4][N:3]=1.C(N(CC)CC)C.[CH3:18][N:19]([CH3:23])[C:20](Cl)=[O:21]>C(Cl)Cl>[CH3:18][N:19]([CH3:23])[C:20]([NH:1][C:2]1[CH:6]=[C:5]([C:7]([CH3:10])([CH3:9])[CH3:8])[NH:4][N:3]=1)=[O:21]

참가 물질

5

반응물 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 5227873-Amino-5-tert-butylpyrazole

생성물 1

HCID 13228710HCID 13228710, 화합물수율 32%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4.2 g of Compound [II] and 3.2 g of triethylamine were dissolved in 50 ml of methylene chloride, and 3.2 g of N,N-dimethylcarbamoyl chloride was added to the solution. The mixture was heated under refluxing and cooled, followed by washing with water. The organic layer was collected, and the solvent was distilled off. The residue was solidified by the addition of a mixed solvent of hexane and benzene. The solid obtained was collected by filtration and dried to obtain 2.0 g of N,N-dimethyl N'-(5-t-butyl-3-pyrazolyl)urea. This compound was recrystallized from hydrous methanol and found to have a melting point of 220° C. to 222° C.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder refluxing
  3. temperaturecooled
  4. washby washing with water
  5. customThe organic layer was collected
  6. distillationthe solvent was distilled off
  7. additionThe residue was solidified by the addition of a mixed solvent of hexane and benzene
  8. customThe solid obtained
  9. filtrationwas collected by filtration
  10. customdried

출처 및 근거

ORD 기록
ord-a283d730f45745da97ab618cabd3929e
출처 데이터셋
uspto-grants-1985_02
특허 번호
US04501606

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