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

HRID 2087013ノート

反応式

HRID 2087013 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=O)[CH:10]([CH2:21][CH3:22])[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.[NH2:24][NH2:25].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:7]=[CH:8][CH:3]=[CH:4][CH:5]=3)=[C:11]([C:13]3[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=3)[NH:25][N:24]=2)=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 9321HydrazineHCID 1353051,3-Propanedione, 2-ethyl-1,3-bis(4-methoxyphenyl)-

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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. HCI, brine, dried, filtered and the solvent was concentrated in vacuo to give the product 4-methoxy-1-[5-(4-methoxyphenyl)-4-benzylpyrazol-3-yl]benzene.

後処理

  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. HCI, brine
  7. customdried
  8. filtrationfiltered
  9. concentrationthe solvent was concentrated in vacuo

出典と根拠

ORDレコード
ord-18ec8cc0d6644fab9433584df70824e5
出典データセット
uspto-grants-2004_04
特許番号
US06727273B2

反応ノート

読み込み中…