Dimethylcarbamoyl Chloride → HCID 13228710、化合物

HRID 615812ノート

反応式

HRID 615812 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 13228710HCID 13228710、化合物収率 32%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a283d730f45745da97ab618cabd3929e
出典データセット
uspto-grants-1985_02
特許番号
US04501606

反応ノート

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