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Formaldehyde → 6-(3-Bromophenyl)-2-hydroxymethyl-3(2H)-pyridazinone

HRID 649132
ノート
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反応式

HRID 649132 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[CH:10][C:11](=[O:14])[NH:12][N:13]=2)[CH:5]=[CH:6][CH:7]=1.[CH2:15]=[O:16]>Cl.CO>[Br:1][C:2]1[CH:3]=[C:4]([C:8]2[CH:9]=[CH:10][C:11](=[O:14])[N:12]([CH2:15][OH:16])[N:13]=2)[CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 712FormaldehydeHCID 128816476-(3-bromophenyl)pyridazin-3(2H)-one

生成物 1

HCID 132358756-(3-Bromophenyl)-2-hydroxymethyl-3(2H)-pyridazinone収率 40%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 887Methanol溶媒

実験手順

2.51 g of 6-(3-bromophenyl)-3(2H)-pyridazinone, 5 ml of a 37% formalin and 2 drops of concentrated hydrochloric acid were dissolved in 50 ml of methanol, and then the solution was heated under reflux for about 7 hours. The mixture was then left to stand overnight, after which it was filtered and the filtrate was concentrated by evaporation under reduced pressure. The resulting residue was extracted with a 1:1 by volume mixture of ethyl acetate and acetone. After distilling the solvent from the extract, there were obtained 1.13 g (yield 40%) of the desired Compound No. 1 in the form of a white solid melting at 228°-229° C.

後処理

  1. temperaturethe solution was heated
  2. temperatureunder reflux for about 7 hours
  3. waitThe mixture was then left
  4. filtrationafter which it was filtered
  5. concentrationthe filtrate was concentrated by evaporation under reduced pressure
  6. extractionThe resulting residue was extracted with a 1:1 by volume mixture of ethyl acetate and acetone
  7. distillationAfter distilling the solvent from the extract

出典と根拠

ORDレコード
ord-832344e5442a482ea22d7fa1ec666e71
出典データセット
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04738961

反応ノート

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