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Sodium Azide → HCID 178476189, 화합물

HRID 2083228
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HRID 2083228 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5]([O:8][CH:9]([C:11]1[CH:12]=[CH:13][C:14]2[O:19][CH:18]=[C:17]([C:20]#[N:21])[C:16](=[O:22])[C:15]=2[CH:23]=1)[CH3:10])(=[O:7])[CH3:6].[N-:24]=[N+:25]=[N-:26].[Na+]>O1CCCC1>[C:5]([O:8][CH:9]([C:11]1[CH:23]=[C:15]2[C:14](=[CH:13][CH:12]=1)[O:19][CH:18]=[C:17]([C:20]1[NH:26][N:25]=[N:24][N:21]=1)[C:16]2=[O:22])[CH3:10])(=[O:7])[CH3:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 33557Sodium AzideHCID 6451240Aluminum(III) ChlorideHCID 203582201-(3-Cyano-4-oxo-4H-1-benzopyran-6-yl)ethyl acetate

생성물 1

HCID 178476189HCID 178476189, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of 45 parts by volume of tetrahydrofuran and 4.005 parts of anyhydrous aluminum chloride there are added 3.86 parts of 6-(1-acetoxyethyl)-4-oxo-4H-1-benzopyran-3-carbonitrile and 2.925 parts of sodium azide, and the resulting mixture is refluxed under stirring for 1.5 hours. After cooling, the solvent is distilled off. To the solid residue are added 2.1 parts of sodium nitrite and ice-water, and the mixture is well shaken. The insoluble material is recovered by filtration and recrystallized from ethyl acetate. The procedure yields 1.88 parts of 6-(1-acetoxyethyl)-3-(1H-tetrazol-5-yl)-chromone as colorless crystals. Melting point: 231°-232° C

후처리

  1. temperaturethe resulting mixture is refluxed
  2. temperatureAfter cooling
  3. distillationthe solvent is distilled off
  4. additionTo the solid residue are added 2.1 parts of sodium nitrite and ice-water
  5. stirringthe mixture is well shaken
  6. filtrationThe insoluble material is recovered by filtration
  7. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-d67c280d70b24789b79193fc546f1ed7
출처 데이터셋
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04085116

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