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Sodium Azide → HCID 178466053, 화합물

HRID 2083234
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HRID 2083234 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5]([C:8]1[CH:9]=[CH:10][C:11]2[O:16][CH:15]=[C:14]([C:17]#[N:18])[C:13](=[O:19])[C:12]=2[CH:20]=1)(=[O:7])[CH3:6].[N-:21]=[N+:22]=[N-:23].[Na+]>O1CCCC1>[C:5]([C:8]1[CH:20]=[C:12]2[C:11](=[CH:10][CH:9]=1)[O:16][CH:15]=[C:14]([C:17]1[NH:23][N:22]=[N:21][N:18]=1)[C:13]2=[O:19])(=[O:7])[CH3:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 33557Sodium AzideHCID 6451240Aluminum(III) ChlorideHCID 137286106-acetyl-4-oxo-4H-1-benzopyran-3-carbonitrile

생성물 1

HCID 178466053HCID 178466053, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To 40 parts by volume of tetrahydrofuran are added under cooling 4.0 parts of anhydrous aluminum chloride, 3.20 parts of 6-acetyl-4-oxo-4H-1-benzopyran-3-carbonitrile and 2.93 parts of sodium azide in the order mentioned and, under stirring, the mixture is refluxed for 30 minutes. After cooled, the reaction mixture is concentrated to dryness. To the residue are added 100 parts by volume of 1N-hydrochloric acid and 3.10 parts of sodium nitrite, and the insoluble material is recovered by filtration and recrystallized four times from dimethylformamide to obtain 0.380 part of 6-acetyl-3-(1H-tetrazol-5-yl)-chromone as colorless crystals.

후처리

  1. temperaturethe mixture is refluxed for 30 minutes
  2. temperatureAfter cooled
  3. concentrationthe reaction mixture is concentrated to dryness
  4. additionTo the residue are added 100 parts by volume of 1N-hydrochloric acid and 3.10 parts of sodium nitrite
  5. filtrationthe insoluble material is recovered by filtration
  6. customrecrystallized four times from dimethylformamide

출처 및 근거

ORD 기록
ord-6138a420df2348cebf0bdae768eb9a17
출처 데이터셋
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04085116

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