Ethanol → Ipriflavone

HRID 1605174

反応式

HRID 1605174 の反応式
O[C:2]1[CH:7]=C(OC(C)C)C=C[C:3]=1[CH:12]([C:19]([CH:21](C1C=CC(OC(C)C)=CC=1O)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:20])C1C=CC=CC=1.[CH:39]([O-])([O-])[O:40][CH2:41][CH3:42].N1CCOC[CH2:46]1.[CH2:51]([OH:53])[CH3:52]>CN(C)C=O>[CH:51]([O:53][C:7]1[CH:42]=[C:41]2[C:12]([C:19](=[O:20])[C:21]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[CH:39][O:40]2)=[CH:3][CH:2]=1)([CH3:46])[CH3:52]

参加物

6

反応物 4

HCID 702EthanolHCID 8083MorpholineHCID 53630039EthylorthoformateHCID 542779182-Hydroxy-4-isopropyloxy-phenyl-benzyl ketone

生成物 1

HCID 3747Ipriflavone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

27 g of 2-hydroxy-4-isopropyloxy-phenyl-benzyl ketone, 22 g of ethyl orthoformate and 5 g of morpholine are boiled for 8 hours in 200 ml of dimethyl formamide. The ethanol formed during the reaction is removed through a fraction head. Then the major part of solvent is distilled off in vacuum and the residue is diluted with dilute aqueous hydrochloric acid. The crude product is filtered and recrystallized from acetone, yielding 24 g of 7-isopropyloxy-isoflavone of m.p. 115°-117°C.

後処理

  1. customis removed through a fraction head
  2. distillationThen the major part of solvent is distilled off in vacuum
  3. additionthe residue is diluted with dilute aqueous hydrochloric acid
  4. filtrationThe crude product is filtered
  5. customrecrystallized from acetone

出典と根拠

ORDレコード
ord-9195dddb56f746f8a95ceb80bded6348
出典データセット
uspto-grants-1976_04
特許番号
US03949085

関連ノート

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