Acetic Acid → 2-(3-Methoxy-2-nitrophenyl)-4H-chromen-4-one

HRID 260086ノート

反応式

HRID 260086 の反応式
C(O)(=O)C.S(=O)(=O)(O)O.O[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17](=[O:32])[CH2:18][C:19]([C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([O:27][CH3:28])[C:22]=1[N+:29]([O-:31])=[O:30])=[O:20]>O>[CH3:28][O:27][C:23]1[C:22]([N+:29]([O-:31])=[O:30])=[C:21]([C:19]2[O:20][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[C:17](=[O:32])[CH:18]=2)[CH:26]=[CH:25][CH:24]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 224024981-(2-Hydroxyphenyl)-3-(3-methoxy-2-nitrophenyl)propane-1,3-dione

生成物 1

HCID 224024972-(3-Methoxy-2-nitrophenyl)-4H-chromen-4-one収率 70.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of glacial acetic acid (15 mL), concentrated sulfuric acid (180 mL), and 1-(2-hydroxy-phenyl)-3-(3-methoxy-2-nitrophenyl)propane -1,3 -dione (770 mg, 2.43 mmol) is heated at reflux for 2.5 hours. The hot solution is poured onto crushed ice and H2O (200 mL), stirring vigorously for 30 minutes. The solution is cooled in a refrigerator. The resulting solid is filtered and washed with H2O to yield 2-(3-methoxy-2-nitrophenyl)-4-oxo-4H-[1]benzopyran (510 mg, 70%) as a brown solid.

後処理

  1. temperatureat reflux for 2.5 hours
  2. additionThe hot solution is poured
  3. temperatureThe solution is cooled in a refrigerator
  4. filtrationThe resulting solid is filtered
  5. washwashed with H2O

出典と根拠

ORDレコード
ord-9639366cc73c4670aed65e75b942fc59
出典データセット
uspto-grants-1996_06
特許番号
US05525625

反応ノート

読み込み中…