Hydrochloric Acid → HCID 10424340、化合物

HRID 1065962

反応式

HRID 1065962 の反応式
[ClH:1].OS(O)(=O)=O.[Na+].[Cl-].[CH3:9][C:10]([C:12]1[CH:13]=[CH:14][C:15]([OH:19])=[C:16]([OH:18])[CH:17]=1)=[O:11].O[C:21]1[CH:28]=[C:27]([OH:29])[CH:26]=[CH:25][C:22]=1[CH:23]=O>C(OCC)(=O)C>[Cl-:1].[OH:18][C:16]1[CH:17]=[C:12]([CH:13]=[CH:14][C:15]=1[OH:19])[C:10]1[CH:9]=[CH:23][C:22]2[C:25](=[CH:26][C:27]([OH:29])=[CH:28][CH:21]=2)[O+:11]=1

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 1118Sulfuric AcidHCID 5234Sodium ChlorideHCID 72132,4-DihydroxybenzaldehydeHCID 145303',4'-Dihydroxyacetophenone

生成物 1

HCID 10424340HCID 10424340、化合物収率 75%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

At 0° C., hydrochloric acid (generated by dropwise addition of H2SO4 to NaCl) was bubbled in a two-necked flask containing 12 g (0.079 mol) of 3,4-dihydroxyacetophenone, 10.88 g (0.079 mol) of 2,4-dihydroxybenzaldehyde and 100 ml of ethyl acetate distilled beforehand. The product started to precipitate after 30 minutes. The bubbling was continued for another 1 hour and then the reaction was stopped. The solution was kept at −18° C. for 3 days and then it was filtered. The filtrate was evaporated and it was taken up in ether; the product precipitated. It was separated from the ether, dissolved in hot methanol and then it was added slowly to an equivalent volume of acetone. The solution was placed in a refrigerator and the product started to precipitate. After filtration, the filtrate was evaporated, dissolved in a minimum of methanol and then ether was added until a precipitate appeared. The procedure was thus repeated several times until precipitate no longer appeared. The purity of the 3′,4′,7-trihydroxyflavylium chloride precipitate thus obtained with a yield of 75% was checked by HPLC (high-performance liquid chromatography).

後処理

  1. customwas bubbled in a two-necked flask
  2. customto precipitate after 30 minutes
  3. waitThe solution was kept at −18° C. for 3 days
  4. filtrationit was filtered
  5. customThe filtrate was evaporated
  6. customthe product precipitated
  7. customIt was separated from the ether
  8. dissolutiondissolved in hot methanol
  9. additionit was added slowly to an equivalent volume of acetone
  10. customto precipitate
  11. filtrationAfter filtration
  12. customthe filtrate was evaporated
  13. dissolutiondissolved in a minimum of methanol
  14. additionether was added until a precipitate

出典と根拠

ORDレコード
ord-cd034231b3244a81ab36790ecbdf8386
出典データセット
uspto-grants-2001_06
特許番号
US06241785B1

関連ノート

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