Hydrochloric Acid → HCID 178515425、化合物

HRID 26661

反応式

HRID 26661 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 178515425HCID 178515425、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7b96c81ffadc464497b8bf34f0ecad9d
出典データセット
uspto-grants-1979_04
特許番号
US04151180

関連ノート

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