Triethylamine → HCID 14624371、化合物

HRID 1650765

反応式

HRID 1650765 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]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15].[CH2:21]([N:23]([CH2:26][CH3:27])[C:24]#[N:25])[CH3:22].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH2:21]([N:23]([C:24]1[N:10]([C:3]2[C:2]([Cl:1])=[CH:7][C:6]([Cl:8])=[CH:5][C:4]=2[Cl:9])[N:11]=[C:12]([C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15])[N:25]=1)[CH2:26][CH3:27])[CH3:22]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 12050DiethylcyanamideHCID 86743923HCID 86743923、化合物

生成物 1

HCID 14624371HCID 14624371、化合物収率 54.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

3.4 g (0.008 mol) of pentafluoropropionyl bromide 2,4,6-trichlorophenylhydrazone and 0.8 g (0.008 mol) of N,N-diethylcyanamide were added to 20 ml of toluene. Then, 0.9 g (0.009 mol) of triethylamine was added thereto under stirring at room temperature. After completion of the dropwise addition, stirring was continued at room temperature for further 1 hour. Then, 20 ml of toluene was added thereto, followed by washing with water. The organic layer was dried, and the solvent was distilled off. The residue was purified by silica gel column chromatography to obtain 1.9 g (yield: 54.3%) of the desired compound as a brown powder. Melting point: 66°-70° C.

後処理

  1. additionAfter completion of the dropwise addition
  2. stirringstirring
  3. washby washing with water
  4. customThe organic 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-4dab9342e66f404f853b7217f76fd96a
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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