Water → Flavokavain A

HRID 364656

反応式

HRID 364656 の反応式
[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([O:10][CH3:11])[C:3]=1[C:12](=[O:14])[CH3:13].[CH3:15][O:16][C:17]1[CH:18]=[CH:19][C:20]([CH:23]=O)=[CH:21][CH:22]=1.[OH-].[K+].O>C(O)C>[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([O:10][CH3:11])[C:3]=1[C:12](=[O:14])[CH:13]=[CH:23][C:20]1[CH:19]=[CH:18][C:17]([O:16][CH3:15])=[CH:22][CH:21]=1

参加物

6

反応物 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 312444-MethoxybenzaldehydeHCID 66654Xanthoxylin

生成物 1

HCID 235736Flavokavain A収率 58%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution containing 196 mg of 2'-hydroxy-4',6'-dimethoxyacetophenone and 150 mg of anisaldehyde in 3 ml of ethanol was added 50% aqueous potassium hydroxide (3 ml). After being stirred at room temperature for 3 days, the mixture was poured into 30 ml of cold water. The mixture was then extracted with three 30 ml portions of ethyl acetate. The combined ethyl acetate extracts were washed with water, dried over anhydrous sodium sulfate and then evaporated under reduced pressure to give a crystalline residue. Recrystallization of the residue from methanol gave 182 mg (50% yield) of 2'-hydroxy-4,4',6'-trimethoxychalcone as yellow needles: m.p. 110.7° C.

後処理

  1. extractionThe mixture was then extracted with three 30 ml portions of ethyl acetate
  2. washThe combined ethyl acetate extracts were washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customevaporated under reduced pressure
  5. customto give a crystalline residue
  6. customRecrystallization of the residue from methanol

出典と根拠

ORDレコード
ord-7b4b85d9d4c8416dbac5f909abb7e2ae
出典データセット
uspto-grants-1986_08
特許番号
US04605674

関連ノート

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