Carbonic acid-guanidine (1:1) → HCID 178468831、化合物

HRID 1617144ノート

反応式

HRID 1617144 の反応式
[C:1](=O)(O)O.[NH2:5][C:6]([NH2:8])=[NH:7].[CH3:9][O:10][C:11](=[O:28])[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][CH:19]([C:23](OCC)=[O:24])[C:20](=O)[CH3:21])[CH:13]=1>CCO>[CH2:9]([O:10][C:11](=[O:28])[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][C:19]2[C:23]([OH:24])=[N:7][C:6]([NH2:8])=[N:5][C:20]=2[CH3:21])[CH:13]=1)[CH3:1]

参加物

4

反応物 2

HCID 286947Carbonic acid-guanidine (1:1)HCID 23005490HCID 23005490、化合物

生成物 1

HCID 178468831HCID 178468831、化合物収率 96.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Guanidine carbonate (2.71 g) was added to a stirred solution of 3-(2-ethoxycarbonyl-3-oxo-butyl)-benzoic acid methyl ester (2.12 g) in EtOH (40 mL). The reaction mixture was heated to reflux for 6 h and allowed to cool. The solvent was evaporated under reduced pressure and the residue suspended in water (30 mL). The resulting precipitate was collected by filtration and the solid suspended in EtOAc (30 mL). The solid was collected by filtration to give the subtitle compound as a colourless solid 2.12 g that was used without further purification.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 6 h
  3. temperatureto cool
  4. customThe solvent was evaporated under reduced pressure
  5. filtrationThe resulting precipitate was collected by filtration
  6. filtrationThe solid was collected by filtration

出典と根拠

ORDレコード
ord-10b99a1bfac1492b9e0aede958da3120
出典データセット
uspto-grants-2014_07
特許番号
US08765939B2

反応ノート

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