2'-Hydroxyacetophenone → 3-Formylchromone

HRID 26658

反応式

HRID 26658 の反応式
[C:1](=[O:3])=O.[CH3:4]C(C)=O.[OH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15](=[O:17])[CH3:16]>CN(C)C=O>[O:17]=[C:15]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[O:8][CH:4]=[C:16]1[CH:1]=[O:3]

参加物

4

反応物 2

HCID 83752'-HydroxyacetophenoneHCID 18522661Acetone cardice

生成物 1

HCID 871123-Formylchromone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In 80 volume parts of dimethylformamide are dissolved 25 parts of orthohydroxyacetophenone and, while the solution is externally cooled to about -20° C. with dry ice-acetone, 80 volume parts of tetrachloropyrophosphoric acid are added dropwise to the solution. The resulting mixture is stirred at room temperature for 13 hours. Then, the reaction mixture is poured into ice water and the resulting crystals are recovered by filtration, washed with water and ethanol and finally recrystallized from acetone. The procedure yields of 4-oxo-4H-1-benzopyran-3-carboxaldehyde as colorless crystals melting at 152°-153° C.

後処理

  1. additionare added dropwise to the solution
  2. filtrationthe resulting crystals are recovered by filtration
  3. washwashed with water and ethanol
  4. customfinally recrystallized from acetone

出典と根拠

ORDレコード
ord-96922e08165340108b55feb1592c051d
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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