Morpholine → 7-Hydroxyisoflavone

HRID 6277

반응식

HRID 6277 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 53768917-Hydroxyisoflavone수율 91.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a8539b47ced44f24996e5458c2287ac2
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05247102

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