Tributyltin azide → HCID 178493528, 화합물

HRID 264060

반응식

HRID 264060 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178493528HCID 178493528, 화합물수율 34.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4b9267ecfe9c4af8b99dc2952925e96e
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05646170

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