Dimethylformamide → 7-Hydroxyisoflavone

HRID 6279

反応式

HRID 6279 の反応式
OC1C=C(O)C=CC=1[CH:9]([C:16]([CH:18]([C:25]1[CH:30]=[CH:29]C(O)=CC=1O)C1C=CC=CC=1)=[O:17])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.CN(C)C=[O:36].N1CCOCC1.[CH2:44]([O:46][CH:47]([O-])[O-])[CH3:45]>C(Cl)(Cl)Cl>[OH:36][C:29]1[CH:45]=[C:44]2[C:18]([C:16](=[O:17])[C:9]([C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=3)=[CH:47][O:46]2)=[CH:25][CH:30]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 8083MorpholineHCID 53630039EthylorthoformateHCID 540149872,4-Dihydroxy-phenyl-benzyl-ketone

生成物 1

HCID 53768917-Hydroxyisoflavone収率 90.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

A mixture of 100 kg (438.5 mole) of 2,4-dihydroxy-phenyl-benzyl-ketone, 38 kg of dimethyl-formamide, 5.2 kg of morpholine and 75 kg (506 mole) of ethyl-orthoformate is stirred at 80°-90° C., while within one hour crystallization is initiated. 360 kg of chloroform are added to the suspension after 7 hours at 60° C. After cooling the crystalline substance is centrifuged, covered with chloroform, filtered and dried. 94.5 kg of 7-hydroxy-isoflavone are obtained, 7-ethoxy-isoflavone content: 0.1% by weight, yield: 90.5%.

後処理

  1. temperatureAfter cooling the crystalline substance
  2. filtrationfiltered
  3. customdried

出典と根拠

ORDレコード
ord-e89dd36c6e3b43d29e69f02bfcdffabb
出典データセット
uspto-grants-1993_09
特許番号
US05247102

関連ノート

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