Triethylamine → HCID 14624341、化合物

HRID 1650764

反応式

HRID 1650764 の反応式
[N+:1]([C:4]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:6][C:5]=1[NH:14][N:15]=[C:16](Br)[C:17]([CH3:20])([CH3:19])[CH3:18])([O-:3])=[O:2].[CH2:22]([N:24]([CH2:27][CH3:28])[C:25]#[N:26])[CH3:23].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH2:22]([N:24]([C:25]1[N:14]([C:5]2[CH:6]=[CH:7][C:8]([C:10]([F:13])([F:12])[F:11])=[CH:9][C:4]=2[N+:1]([O-:3])=[O:2])[N:15]=[C:16]([C:17]([CH3:20])([CH3:19])[CH3:18])[N:26]=1)[CH2:27][CH3:28])[CH3:23]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 12050DiethylcyanamideHCID 86743922HCID 86743922、化合物

生成物 1

HCID 14624341HCID 14624341、化合物収率 84.4%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

7.4 g (0.02 mol) of 2,2-dimethylpropionyl bromide 2-nitro-4-trifluoromethylphenylhydrazone and 2.0 g (0.02 mol) of N,N-diethylcyanamide were added to 100 ml of toluene. Then, 2.2 g (0.022 mol) of triethylamine was dropwise added under stirring at room temperature. After completion of the dropwise addition, stirring was continued at room temperature for further 1 hour. Then, 100 ml of toluene was added and washed with water. The organic layer was dried, and the solvent was distilled off. The residue was purified by silica gel column chromatography to obtain 6.5 g (yield: 84.4%) of the desired compound as a pale yellow liquid. Refractive index nD20 : 1.4911.

後処理

  1. additionAfter completion of the dropwise addition
  2. stirringstirring
  3. washwashed 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-4eb6eb4f9ae149d9bf2610c10b131d30
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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