Triethylamine → HCID 14624380, 화합물

HRID 1650769

반응식

HRID 1650769 반응식
[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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 119415MethylcyanamideHCID 85583792HCID 85583792, 화합물

생성물 1

HCID 14624380HCID 14624380, 화합물수율 85%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d072e7ff386c4e34ba5de1a214e59b4f
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04925864

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