Water → HCID 14304992, 화합물

HRID 2050683노트

반응식

HRID 2050683 반응식
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

참가 물질

5

반응물 3

HCID 962Water2회HCID 25134Boron tribromideHCID 143049774-Oxo-2-(3,4,5-trimethoxyphenyl)-4H-1-benzopyran-3-carboxylic acid

생성물 1

HCID 14304992HCID 14304992, 화합물수율 85%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-26024188fb0b42ddb58631608b83297b
출처 데이터셋
uspto-grants-1991_05
특허 번호
US05013852

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