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Keto-pantoyllactone → 3,4-diamino-6-(1',1'-dimethyl-2'-hydroxyethyl)-1,2,4,-triazin-5(4H)-one hydrochloride

HRID 843608
ノート
印刷プレビュー

反応式

HRID 843608 の反応式
[CH3:1][C:2]1([CH3:9])[CH2:6][O:5][C:4](=[O:7])[C:3]1=O.[ClH:10].[NH2:11][NH:12][C:13]([NH:15][NH2:16])=[NH:14].O>C(O)C>[ClH:10].[NH2:14][C:13]1[N:15]([NH2:16])[C:4](=[O:7])[C:3]([C:2]([CH3:9])([CH3:1])[CH2:6][OH:5])=[N:11][N:12]=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 3

HCID 39Keto-pantoyllactoneHCID 962WaterHCID 178479531HCID 178479531、化合物

生成物 1

HCID 226111153,4-diamino-6-(1',1'-dimethyl-2'-hydroxyethyl)-1,2,4,-triazin-5(4H)-one hydrochloride収率 61%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Dihydro-4,4-dimethyl-2,3-furandione (2 g, 15.6 mmole) and 1,3-diaminoguanidine monohydrochloride (12.96 g, 15.61 mmole) were dissolved in ethanol and the resulting solution heated to reflux temperatures. To the refluxing reaction mixture, was added water until a clear solution was obtained. The mixture was then refluxed overnight, cooled to room temperature and stored at −20° C. overnight. The product which separated was filtered and dried. It was crystallized from a mixture of ethanol and water to give 3,4-diamino-6-(1′,1′-dimethyl-2′-hydroxyethyl)-1,2,4-triazin-5(4H)-one hydrochloride (2.24 g, 61%), m.p. 221-222° C. (dec).

後処理

  1. temperaturethe resulting solution heated
  2. temperatureto reflux temperatures
  3. customTo the refluxing reaction mixture
  4. customwas obtained
  5. temperatureThe mixture was then refluxed overnight
  6. customThe product which separated
  7. filtrationwas filtered
  8. customdried
  9. customIt was crystallized from a mixture of ethanol and water

出典と根拠

ORDレコード
ord-862067304a844252aa24074a14206b26
出典データセット
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06380192B1

反応ノート

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