Morpholine → 7-Hydroxyisoflavone

HRID 6277

反応式

HRID 6277 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.N1CC[O:36]CC1.[CH2:39]([O:41][CH:42]([O-])[O-])[CH3:40]>CN(C)C=O>[OH:36][C:29]1[CH:40]=[C:39]2[C:18]([C:16](=[O:17])[C:9]([C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=3)=[CH:42][O:41]2)=[CH:25][CH:30]=1

参加物

5

反応物 3

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

生成物 1

HCID 53768917-Hydroxyisoflavone収率 91.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

50 g (0.219 mole) of a mixture of 2,4-dihydroxy-phenyl-benzyl-ketone, 20 ml of dimethyl-formamide, 2.6 ml of morpholine and 39.06 g (0.26 mole) of ethyl-orthoformate is stirred for 7 hours at 80°-90° C. After 25 minutes crystallization can be observed. At the end of the reaction time the crystallized suspension is diluted with 120 ml of chloroform and it is crystallized at 0° C. for 2 hours. After filtration the product is covered twice with 45 ml of chloroform and dried. 47.9 g of 7-hydroxy-isoflavone are obtained.

後処理

  1. customAfter 25 minutes crystallization
  2. additionAt the end of the reaction time the crystallized suspension is diluted with 120 ml of chloroform and it
  3. customis crystallized at 0° C. for 2 hours
  4. filtrationAfter filtration the product
  5. customdried

出典と根拠

ORDレコード
ord-a8539b47ced44f24996e5458c2287ac2
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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