Hexane → 4-phenyl-1H-1,2,3-triazole

HRID 1764079ノート

反応式

HRID 1764079 の反応式
[C:1]1([C:7]#[CH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Si]([N:13]=[N+:14]=[N-:15])(C)(C)C.CCCCCC>CCOCC>[C:1]1([C:7]2[N:13]=[N:14][NH:15][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 8058HexaneHCID 10821PhenylacetyleneHCID 78378Azidotrimethylsilane

生成物 1

HCID 1784201274-phenyl-1H-1,2,3-triazole収率 76.3%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
150 °C

実験手順

##STR9## Phenylethyne (12.0 g) and Me3SiN3 (7.8 g) were sealed into a heavy-walled glass reactor at -70° C. and 0.6 mm Hg. The mixture was heated at 150° C. for 10 hrs., cooled, and dissolved in Et2O. The Et2O was treated exactly as in Example 2, reduced to 100 ml total volume, a little hexane added and chilled in a refrigerator overnight. Filtration gave 7.5 g (76%) white crystals mp 146.9-149.0.

後処理

  1. temperature, cooled
  2. temperaturechilled in a refrigerator overnight
  3. filtrationFiltration

出典と根拠

ORDレコード
ord-5a5dc2fb2cda4cd2bb2d3c6eeab48b27
出典データセット
uspto-grants-1978_09
特許番号
US04115288

反応ノート

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