4-Phenyl-3-butyn-2-one → HCID 178467506, 화합물

HRID 1605001노트

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HRID 1605001 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178467506HCID 178467506, 화합물수율 28%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
140 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f2185ea8cde04abfa1f50b48c71660f9
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03948932

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