4-Phenyl-3-butyn-2-one → HCID 178467506、化合物

HRID 1604998ノート

反応式

HRID 1604998 の反応式
[C:1]([C:4]#[C:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)(=[O:3])[CH3:2].C[Si]([N:16]=[N+:17]=[N-:18])(C)C>CCOCC>[C:1]([C:4]1[N:16]=[N:17][NH:18][C:5]=1[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 745554-Phenyl-3-butyn-2-oneHCID 78378Azidotrimethylsilane

生成物 1

HCID 178467506HCID 178467506、化合物収率 28%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
140 °C

実験手順

A mixture of 30 g (0.21 mole) of acetylphenyl-acetylene and 24 g (0.21 mole) of trimethylsilyl azide was heated at 140°C for 24 hours. It was then cooled, dissolved in ether, and extracted with dilute sodium hydroxide. This aqueous layer was separated and made acidic with dilute HCl. The precipitate was recrystallized from benzene-petroleum ether to give 11 g (28%) of 4-acetyl-5-phenyltriazole, m.p. 117°-118°C.

後処理

  1. temperatureIt was then cooled
  2. extractionextracted with dilute sodium hydroxide
  3. customThis aqueous layer was separated
  4. customThe precipitate was recrystallized from benzene-petroleum ether

出典と根拠

ORDレコード
ord-208daa7bc6674a70a9370a464c2a0e47
出典データセット
uspto-grants-1976_04
特許番号
US03948929

反応ノート

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