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

HRID 1283789노트

반응식

HRID 1283789 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-0798df346f6649fa8ca7dd510fd34f9b
출처 데이터셋
uspto-grants-1976_08
특허 번호
US03976633

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