Hydrochloric Acid → 4-Oxo-4H-chromene-3-carbonitrile

HRID 26659

反応式

HRID 26659 の反応式
[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH:4]=[C:3]1[CH:12]=O.Cl.[NH2:15]O.Cl>C(O)C>[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH:4]=[C:3]1[C:12]#[N:15]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 871123-FormylchromoneHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 5212984-Oxo-4H-chromene-3-carbonitrile

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2.52 Parts of 4-oxo-4H-1-benzopyran-3-carboxaldehyde are admixed well with 2.10 parts of hydroxylamine hydrochloride, followed by the addition of 30 volume parts of 95 weight % ethyl alcohol and 0.5 volume part of concentrated hydrochloric acid. The whole mixture is refluxed for 6 hours and cooled. The resulting precipitate is recovered by filtration, treated with activated carbon and recrystallized from ethanol. This procedure yields 4-oxo-4H-1-benzopyran-3-carbonitrile as colorless crystals. Melting point: 177°-178° C.

後処理

  1. temperatureThe whole mixture is refluxed for 6 hours
  2. temperaturecooled
  3. filtrationThe resulting precipitate is recovered by filtration
  4. additiontreated with activated carbon
  5. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-a98eeec6f3a04f918a3cb048838d6113
出典データセット
uspto-grants-1979_04
特許番号
US04151180

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