4-Methoxynaphthalen-1-ylmethylamine → 4-Chloro-5-(4-methoxy-1-naphthylmethylamino)-3(2H)pyridazinone

HRID 1085791

反応式

HRID 1085791 の反応式
[Cl:1][C:2]1[C:3](=[O:9])[NH:4][N:5]=[CH:6][C:7]=1Cl.[CH3:10][O:11][C:12]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:15]([CH2:22][NH2:23])=[CH:14][CH:13]=1>C(O)C>[Cl:1][C:2]1[C:3](=[O:9])[NH:4][N:5]=[CH:6][C:7]=1[NH:23][CH2:22][C:15]1[C:16]2[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:12]([O:11][CH3:10])=[CH:13][CH:14]=1

参加物

4

反応物 2

HCID 591394-Methoxynaphthalen-1-ylmethylamineHCID 732474,5-Dichloro-3-hydroxypyridazine

生成物 1

HCID 150071864-Chloro-5-(4-methoxy-1-naphthylmethylamino)-3(2H)pyridazinone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture comprising 330 mg of 4,5-dichloro-3(2H)pyridazinone, 1.12 g of 4-methoxy-1-naphthylmethylamine and 30 ml of ethanol, was refluxed under stirring overnight. The solvent was evaporated under reduced pressure, and a mixture of ethyl acetate and ethyl ether was poured to the residue, whereupon precipitated crystals were collected by filtration. The product was recrystallized from a mixture of methanol/water to obtain 410 mg of the above identified command as slightly yellow crystals having a melting point of from 265° to 266° C.

後処理

  1. temperaturewas refluxed
  2. customThe solvent was evaporated under reduced pressure
  3. additiona mixture of ethyl acetate and ethyl ether
  4. additionwas poured to the residue
  5. customwhereupon precipitated crystals
  6. filtrationwere collected by filtration
  7. customThe product was recrystallized from a mixture of methanol/water
  8. customto obtain 410 mg of the
  9. customof from 265° to 266° C.

出典と根拠

ORDレコード
ord-0f9cad209219493591eddaa88cca1417
出典データセット
uspto-grants-1991_04
特許番号
US05011839

関連ノート

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