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

HRID 1085797

반응식

HRID 1085797 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 98847584,6-Dichloro-5-(4-methoxy-1-naphthylmethylamino)-3(2H)pyridazinone

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-f83b4264c56b4aef9b9b6fb6f5dcebcc
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05011839

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