4-Methoxynaphthalen-1-ylmethylamine → 4,6-Dichloro-5-(4-methoxy-1-naphthylmethylamino)-3(2H)pyridazinone

HRID 1085797

反応式

HRID 1085797 の反応式
[Cl:1][C:2]1[C:3](=[O:10])[NH:4][N:5]=[C:6]([Cl:9])[C:7]=1Cl.[CH3:11][O:12][C:13]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16]([CH2:23][NH2:24])=[CH:15][CH:14]=1>C(O)C>[Cl:1][C:2]1[C:3](=[O:10])[NH:4][N:5]=[C:6]([Cl:9])[C:7]=1[NH:24][CH2:23][C:16]1[C:17]2[C:22](=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:13]([O:12][CH3:11])=[CH:14][CH:15]=1

参加物

4

反応物 2

HCID 591394-Methoxynaphthalen-1-ylmethylamineHCID 111063493,4,5-Trichlor-6-hydroxypyridazin

生成物 1

HCID 98847584,6-Dichloro-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 800 mg of 4,5,6-trichloro-3(2H)pyridazinone, 2.68 g of 4-methoxy-1-naphthylmethylamine and 10 ml of ethanol, was refluxed under stirring for 4 hours. After cooling, precipitated crystals were collected by filtration. Then, the product was dissolved in hot ethyl acetate and treated by silica gel. The filtrate was concentrated, and precipitated crystals were collected by filtration to obtain 330 mg of the above identified compound as colorless crystals having a melting point of from 228° to 231° C.

後処理

  1. temperaturewas refluxed
  2. temperatureAfter cooling
  3. customprecipitated crystals
  4. filtrationwere collected by filtration
  5. dissolutionThen, the product was dissolved in hot ethyl acetate
  6. additiontreated by silica gel
  7. concentrationThe filtrate was concentrated
  8. customprecipitated crystals
  9. filtrationwere collected by filtration
  10. customto obtain 330 mg of the
  11. customof from 228° to 231° C.

出典と根拠

ORDレコード
ord-f83b4264c56b4aef9b9b6fb6f5dcebcc
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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