Acetyl chloride → 3-Acetyl-1,3-bis(2-cyano-5-trifluoromethylphenyl)triazene

HRID 1283789ノート

反応式

HRID 1283789 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:4]=1[N:13]=[N:14][NH:15][C:16]1[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[CH:18][C:17]=1[C:26]#[N:27])#[N:2].[H-].[Na+].[C:30](Cl)(=[O:32])[CH3:31]>CCOCC>[C:30]([N:13]([C:4]1[CH:5]=[C:6]([C:9]([F:12])([F:11])[F:10])[CH:7]=[CH:8][C:3]=1[C:1]#[N:2])[N:14]=[N:15][C:16]1[CH:21]=[C:20]([C:22]([F:23])([F:24])[F:25])[CH:19]=[CH:18][C:17]=1[C:26]#[N:27])(=[O:32])[CH3:31]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 24758Sodium hydrideHCID 30354951,3-Bis(2-cyano-5-(trifluoromethyl)phenyl)triazene

生成物 1

HCID 215163803-Acetyl-1,3-bis(2-cyano-5-trifluoromethylphenyl)triazene

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of 5.6 g. (0.015 mol.) of 1,3-bis(2-cyano-5-trifluoromethylphenyl)triazene in 450 ml. of warm ether is added dropwise to a slurry of 1.20 g. (0.025 mol.) of 50% sodium hydride in 15 ml. of ether. Upon cessation of gas evolution, 1.42 g. (0.018 mol.) of acetyl chloride is gradually added and the reaction mixture is stirred for two hours at 25°. The mixture is filtered to remove excess sodium hydride and the filtrate is concentrated to give 3-acetyl-1,3-bis(2-cyano-5-trifluoromethylphenyl)triazene, m.p. 111°-112° (hexane).

後処理

  1. filtrationThe mixture is filtered
  2. customto remove excess sodium hydride
  3. concentrationthe filtrate is concentrated

出典と根拠

ORDレコード
ord-0798df346f6649fa8ca7dd510fd34f9b
出典データセット
uspto-grants-1976_08
特許番号
US03976633

反応ノート

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