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2-ethyl-4,5,6-trichloro-3(2H)pyridazinone → 2-ethyl-4,6-dichloro-5-(3-n-propoxy-4-methoxybenzylamino)-3(2H)pyridazinone

HRID 1111139
ノート
印刷プレビュー

反応式

HRID 1111139 の反応式
[CH2:1]([N:3]1[C:8](=[O:9])[C:7]([Cl:10])=[C:6](Cl)[C:5]([Cl:12])=[N:4]1)[CH3:2].[CH2:13]([O:16][C:17]1[CH:18]=[C:19]([CH:22]=[CH:23][C:24]=1[O:25][CH3:26])[CH2:20][NH2:21])[CH2:14][CH3:15]>C(O)C>[CH2:1]([N:3]1[C:8](=[O:9])[C:7]([Cl:10])=[C:6]([NH:21][CH2:20][C:19]2[CH:22]=[CH:23][C:24]([O:25][CH3:26])=[C:17]([O:16][CH2:13][CH2:14][CH3:15])[CH:18]=2)[C:5]([Cl:12])=[N:4]1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 140323942-ethyl-4,5,6-trichloro-3(2H)pyridazinoneHCID 150790273-n-Propoxy-4-methoxybenzylamine

生成物 1

HCID 150790872-ethyl-4,6-dichloro-5-(3-n-propoxy-4-methoxybenzylamino)-3(2H)pyridazinone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture comprising 455 mg of 2-ethyl-4,5,6-trichloro-3(2H)pyridazinone, 1.20 g of 3-n-propoxy-4-methoxybenzylamine and 20 ml of ethanol, was refluxed under stirring for 3.5 hours. Ethanol was distilled off under reduced pressure, and water was poured into the residue thereby obtained. The mixture was extracted with ethyl acetate. The extract was washed with dilute hydrochloric acid and water in this order and dried over sodium sulfate. Then, the solvent was distilled off to obtain a light brown viscous oily substance. The product was purified by silica gel column chromatography by using a solvent mixture of benzene-ethyl acetate (15:1 v/v) as the eluent, to obtain 277 mg of the above identified compound. The physical properties and the spectrum data of NMR and MS of the compound completely agreed to those of the compound prepared by the method (1).

後処理

  1. temperaturewas refluxed
  2. distillationEthanol was distilled off under reduced pressure, and water
  3. additionwas poured into the residue
  4. customthereby obtained
  5. extractionThe mixture was extracted with ethyl acetate
  6. washThe extract was washed with dilute hydrochloric acid and water in this order
  7. dry with materialdried over sodium sulfate
  8. distillationThen, the solvent was distilled off
  9. customto obtain a light brown viscous oily substance
  10. customThe product was purified by silica gel column chromatography
  11. additiona solvent mixture of benzene-ethyl acetate (15:1 v/v) as the eluent
  12. customto obtain 277 mg of the
  13. customprepared by the method (1)

出典と根拠

ORDレコード
ord-569ae31ff6b840e18f4f5349752fc322
出典データセット
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04978665

反応ノート

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