Triethylamine → HCID 14624380、化合物

HRID 1650769

反応式

HRID 1650769 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[NH:10][N:11]=[C:12](Br)[C:13]([CH3:16])([CH3:15])[CH3:14].[CH3:18][NH:19][C:20]#[N:21].C(N(CC)CC)C>C1(C)C=CC=CC=1>[C:13]([C:12]1[N:21]=[C:20]([NH:19][CH3:18])[N:10]([C:3]2[C:2]([Cl:1])=[CH:7][C:6]([Cl:8])=[CH:5][C:4]=2[Cl:9])[N:11]=1)([CH3:16])([CH3:15])[CH3:14]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 119415MethylcyanamideHCID 85583792HCID 85583792、化合物

生成物 1

HCID 14624380HCID 14624380、化合物収率 85%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

3.6 g (0.01 mol) of 2,2-dimethylpropionyl bromide 2,4,6-trichlorophenylhydrazone and 0.6 g (0.01 mol) of N-methylcyanamide were added to 50 ml of toluene. Then, 1.1 g (0.011 mol) of triethylamine was dropwise added under stirring at room temperature. After the dropwise addition, stirring was continued at the same temperature for further 1 hour. After washing the reaction mixture with water, the toluene layer was dried, and the solvent was distilled off. The residue was purified by silica gel column chromatography to obtain 2.8 g (yield: 85%) of 3-(tert-butyl)-5-(N-methylamino)-1-(2,4,6-trichlorophenyl)-1H-1,2,4-triazole as power having a melting point of from 165° to 166° C.

後処理

  1. additionAfter the dropwise addition
  2. stirringstirring
  3. washAfter washing the reaction mixture with water
  4. dry with materialthe toluene layer was dried
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-d072e7ff386c4e34ba5de1a214e59b4f
出典データセット
uspto-grants-1990_05
特許番号
US04925864

関連ノート

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