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Sodium Chloride → 3-Amino-2-imino-6-methyl-2,3-dihydropyrimidin-4(1H)-one

HRID 591221
ノート
印刷プレビュー

反応式

HRID 591221 の反応式
CC[O-].[Na+].[Na].[C:6]([NH:9][NH2:10])([NH2:8])=[NH:7].Cl.[Na+].[Cl-].O=[C:15]([CH3:22])[CH2:16][C:17](OCC)=[O:18]>C(O)C>[NH2:7][C:6]1[N:9]([NH2:10])[C:17](=[O:18])[CH:16]=[C:15]([CH3:22])[N:8]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 5234Sodium ChlorideHCID 8868Ethyl AcetoacetateHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 178418668HCID 178418668、化合物

生成物 1

HCID 9131753-Amino-2-imino-6-methyl-2,3-dihydropyrimidin-4(1H)-one

試薬・触媒・溶媒 1

HCID 702

反応条件

温度
50 °C

実験手順

To a stirring solution of NaOEt prepared from sodium (FLUKA, 9.19 g, 400 mmol) and ethanol (350 mL) was added aminoguanidine hydrochloride (ALDRICH, 44.2 g, 400 mmol). The reaction mixture was heated at 50° C. for 30 min. Then, the mixture was filtered to remove NaCl, and ethyl 3-oxobutanoate (ALDRICH, 25.3 mL, 200 mmol) was added to the filtrate. The reaction mixture was heated under reflux for 5 h and, then, stirred at room temperature overnight. The precipitate obtained was filtered and dried under vacuum to afford Intermediate 1 as a pale pink solid.

後処理

  1. filtrationThen, the mixture was filtered
  2. additionwas added to the filtrate
  3. temperatureThe reaction mixture was heated
  4. temperatureunder reflux for 5 h
  5. customThe precipitate obtained
  6. filtrationwas filtered
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-14cd1255a38d4f75999a61648930ba35
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09238653B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート
Ethanol
溶媒