Hydrochloric Acid → 4-Methoxy-1-[5-(4-methoxyphenyl)4benzylpyrazol-3-yl]benzene

HRID 1767426노트

반응식

HRID 1767426 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=O)[CH:10]([CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:11]([C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=2)=O)=[CH:5][CH:4]=1.[NH2:29][NH2:30].Cl>C(O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:10]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[C:11]([C:13]3[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=3)[NH:30][N:29]=2)=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 9321HydrazineHCID 227255101,3-Bis(4-methoxyphenyl)-2-benzylpropane-1,3-dione

생성물 1

HCID 227256094-Methoxy-1-[5-(4-methoxyphenyl)4benzylpyrazol-3-yl]benzene

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of the 1,3-diketone obtained in step 1 (1.0 equiv.), hydrazine (3.0 equiv.), conc. HCl aq. (catalytic amount) and ethanol was heated to reflux overnight. Cooled to rt and removed solvent in vacuo. Water and ethyl acetate were added. The organic layer was separated, washed with dil. HCl, brine, dried, filtered and the solvent was concentrated in vacuo to give the product 4-methoxy-1-[5-(4-methoxyphenyl)4benzylpyrazol-3-yl]benzene.

후처리

  1. temperaturewas heated
  2. temperatureto reflux overnight
  3. customremoved solvent in vacuo
  4. additionWater and ethyl acetate were added
  5. customThe organic layer was separated
  6. washwashed with dil. HCl, brine
  7. customdried
  8. filtrationfiltered
  9. concentrationthe solvent was concentrated in vacuo

출처 및 근거

ORD 기록
ord-e5022598b46349d794ec824f0ab9f29b
출처 데이터셋
uspto-grants-2007_06
특허 번호
USRE039708E1

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