Tributyltin azide → HCID 178493528、化合物

HRID 264060ノート

反応式

HRID 264060 の反応式
[C:1]([CH:3]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH2:4][C:5]([NH:7][C:8]1[C:13]([O:14][CH3:15])=[CH:12][C:11]([O:16][CH3:17])=[CH:10][C:9]=1[O:18][CH3:19])=[O:6])#[N:2].C([Sn]([N:39]=[N+:40]=[N-:41])(CCCC)CCCC)CCC>O1CCOCC1>[NH:39]1[C:1]([CH:3]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH2:4][C:5]([NH:7][C:8]2[C:9]([O:18][CH3:19])=[CH:10][C:11]([O:16][CH3:17])=[CH:12][C:13]=2[O:14][CH3:15])=[O:6])=[N:2][N:41]=[N:40]1

参加物

4

反応物 2

HCID 4984872Tributyltin azideHCID 86748282beta-cyano-N-(2,4,6-trimethoxyphenyl)benzene propanamide

生成物 1

HCID 178493528HCID 178493528、化合物収率 34.2%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a suspension of the material from step (a) (5.1 g, 0.016 mol) in dioxane (150 mL) at room temperature was added tri-n-butyltin azide (9.36 g, 0.016 mol) under N2 with stirring. The resulting solution was heated to reflux for 24 hours. The solution was then cooled and concentrated in vacuo. The residue was redissolved in ether and HCl gas was then passed through the solution for 30 minutes. This was then concentrated in vacuo to give β-(1H-tetrazol-5-yl)-N-(2,4,6-trimethoxyphenyl)benzene propanamide as a white solid (2.1 g) which was used without further purification.

後処理

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux for 24 hours
  3. temperatureThe solution was then cooled
  4. concentrationconcentrated in vacuo
  5. dissolutionThe residue was redissolved in ether
  6. concentrationThis was then concentrated in vacuo

出典と根拠

ORDレコード
ord-4b9267ecfe9c4af8b99dc2952925e96e
出典データセット
uspto-grants-1997_07
特許番号
US05646170

反応ノート

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