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Phenylglyoxylic acid hydrazide-2-acetylhydrazone → Metamitron

HRID 1077093
ノート
印刷プレビュー

反応式

HRID 1077093 の反応式
[C:1]([NH:4][N:5]=[C:6]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:7]([NH:9][NH2:10])=[O:8])(=O)[CH3:2]>C(O)C>[NH2:10][N:9]1[C:7](=[O:8])[C:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:5][N:4]=[C:1]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

3

反応物 1

HCID 92518Phenylglyoxylic acid hydrazide-2-acetylhydrazone

生成物 1

HCID 38854Metamitron収率 76%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

175 g (0.8 mol) of phenylglyoxylic acid hydrazide-2-acetylhydrazone were dissolved in 2 liters of ethanol and the solution was heated to boil under reflux for 12 hours. After cooling, the product which had precipitated was filtered off. The mother liquor was partially freed from the solvent; on cooling, a further precipitate was obtained, which was also filtered off and well washed with water. The combined precipitates were dried. 123 g (76% of theory) of 4-amino-3-methyl-6-phenyl-1,2,4-triazin-5-(4H)-one of melting point 160°-163°C. were obtained.

後処理

  1. temperaturethe solution was heated
  2. temperatureunder reflux for 12 hours
  3. temperatureAfter cooling
  4. customthe product which had precipitated
  5. filtrationwas filtered off
  6. temperatureon cooling
  7. customa further precipitate was obtained
  8. filtrationwhich was also filtered off
  9. washwell washed with water
  10. customThe combined precipitates
  11. customwere dried

出典と根拠

ORDレコード
ord-72eb00a67aea4d1995ab2d1f8e820036
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03959372

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート