1H-Pyrazole, 4,5-dihydro-3-methyl-5-phenyl- → HCID 19873525、化合物

HRID 465282ノート

反応式

HRID 465282 の反応式
[CH3:1][N:2]([O:21][CH3:22])[S:3]([N:6]([S:8]([NH:11][C:12](=O)[O:13]C1C=CC=CC=1)(=[O:10])=[O:9])[CH3:7])(=[O:5])=[O:4].[CH3:23][C:24]1[CH2:28][CH:27]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[NH:26][N:25]=1>C1C=CC=CC=1>[CH3:1][N:2]([O:21][CH3:22])[S:3]([N:6]([S:8]([NH:11][C:12]([N:26]1[CH:27]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH2:28][C:24]([CH3:23])=[N:25]1)=[O:13])(=[O:9])=[O:10])[CH3:7])(=[O:5])=[O:4]

参加物

4

反応物 2

HCID 101301011H-Pyrazole, 4,5-dihydro-3-methyl-5-phenyl-HCID 19873523HCID 19873523、化合物

生成物 1

HCID 19873525HCID 19873525、化合物収率 42.4%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture comprising 1 g (2.83 mmol) of phenyl N-[(N-(N-methyl-N-methoxyaminosulfonyl)-N-methylamino)sulfonyl]-carbamate, 0.45 g (2.81 mmol) of 3-methyl-5-phenyl-2-pyrazoline and 30 ml of dry benzene was heated at 80° C. for 5 minutes. The mixture was left to cool, and then the solvent was distilled off under reduced pressure. The residue was purified by reverse phase column chromatography (CH3CN: H2O=7:3) to obtain 0.5 g of the desired 1-[(N-(N-methyl-N-methoxyaminosulfonyl)-N-methyl-amino)sulfonylcarbamoyl]-3-methyl-5-phenyl-2-pyrazoline as glassy substance.

後処理

  1. waitThe mixture was left
  2. temperatureto cool
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by reverse phase column chromatography (CH3CN: H2O=7:3)

出典と根拠

ORDレコード
ord-f2648dc302094aa992468d9ac0ed9dba
出典データセット
uspto-grants-1992_10
特許番号
US05152824

反応ノート

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