Water → HCID 14304992、化合物

HRID 477063ノート

反応式

HRID 477063 の反応式
C[O:2][C:3]1[CH:4]=[C:5]([CH:20]=[C:21]([O:25]C)[C:22]=1[O:23]C)[C:6]1[O:7][C:8]2[C:13]([C:14](=[O:19])[C:15]=1[C:16]([OH:18])=[O:17])=[CH:12][CH:11]=[CH:10][CH:9]=2.B(Br)(Br)Br.O>ClCCl>[OH:25][C:21]1[CH:20]=[C:5]([CH:4]=[C:3]([OH:2])[C:22]=1[OH:23])[C:6]1[O:7][C:8]2[C:13]([C:14](=[O:19])[C:15]=1[C:16]([OH:18])=[O:17])=[CH:12][CH:11]=[CH:10][CH:9]=2

参加物

5

反応物 3

HCID 962Water2 回HCID 25134Boron tribromideHCID 143049774-Oxo-2-(3,4,5-trimethoxyphenyl)-4H-1-benzopyran-3-carboxylic acid

生成物 1

HCID 14304992HCID 14304992、化合物収率 85%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

4.0 g of 3',4',5'-trimethoxyflavone-3-carboxylic acid were added to 200 ml of absolute dichloromethane and reacted with 82 ml of a 1 molar boron tribromide solution in absolute dichloromethane under a nitrogen atmosphere at 0° C. The reaction mixture was stirred for twelve hours during which it was allowed to warm to room temperature. Then, for working up, water was carefully added under ice cooling, then made up to twice the volume with water and intensively stirred. The resulting 3',4',5'-trihydroxyflavone-3-carboxylic acid precipitated and was filtered out. The filter cake was washed with water several times and recrystallized from methanol. 3 g of pure 3',4',5'-trihydroxyflavone-3-carboxylic acid were obtained.

後処理

  1. stirringintensively stirred
  2. customThe resulting 3',4',5'-trihydroxyflavone-3-carboxylic acid precipitated
  3. filtrationwas filtered out
  4. washThe filter cake was washed with water several times
  5. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-ba6229479aa04f53b7f9cc7803868a3c
出典データセット
uspto-grants-1989_12
特許番号
US04886806

反応ノート

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