Hydrochloric Acid → HCID 178515425, 화합물

HRID 26661

반응식

HRID 26661 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[O:5]=[C:6]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[O:9][CH:8]=[C:7]1[C:16]#[N:17].[N-:18]=[N+:19]=[N-:20].[Na+].Cl>O1CCCC1>[NH:18]1[C:16]([C:7]2[C:6](=[O:5])[C:11]3[C:10](=[CH:15][CH:14]=[CH:13][CH:12]=3)[O:9][CH:8]=2)=[N:17][N:20]=[N:19]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 33557Sodium AzideHCID 5212984-Oxo-4H-chromene-3-carbonitrileHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 178515425HCID 178515425, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To 100 volume parts of dry tetrahydrofuran are added 4.28 parts of comminuted anhydrous aluminum chloride, 2.50 parts of 4-oxo-4H-1-benzopyran-3-carbonitrile and 4.18 parts of sodium azide in this order and, the whole mixture is refluxed under stirring for 23 hours. Then, to the resulting mixture 35 volume parts of 15 weight% hydrochloric acid are added, followed by distilling off tetrahydrofuran under reduced pressure. The resulting solid residue is recovered by filtration and recrystallized from dimethylformamide. This procedure yields 3-(1H-tetrazol-5-yl) chromone as colorless hairy needles. Melting point: 284°-285° C.(decomp. with foaming).

후처리

  1. temperaturethe whole mixture is refluxed
  2. distillationby distilling off tetrahydrofuran under reduced pressure
  3. filtrationThe resulting solid residue is recovered by filtration
  4. customrecrystallized from dimethylformamide

출처 및 근거

ORD 기록
ord-7b96c81ffadc464497b8bf34f0ecad9d
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151180

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