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Hydrochloric Acid → (1E)-1-[amino-(2,4,6-trichloroanilino)methylidene]-2-methylguanidine;hydrochloride

HRID 1973121
ノート
印刷プレビュー

反応式

HRID 1973121 の反応式
[Cl:1][C:2]1[CH:8]=[C:7]([Cl:9])[CH:6]=[C:5]([Cl:10])[C:3]=1[NH2:4].[CH3:11][NH:12][C:13]([NH:15][C:16]#[N:17])=[NH:14].Cl>C(O)CCC>[ClH:1].[Cl:1][C:2]1[CH:8]=[C:7]([Cl:9])[CH:6]=[C:5]([Cl:10])[C:3]=1[NH:4][C:16]([NH:15][C:13]([NH:12][CH3:11])=[NH:14])=[NH:17]
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 313Hydrochloric AcidHCID 124712,4,6-TrichloroanilineHCID 178485119HCID 178485119、化合物

生成物 1

HCID 178485125(1E)-1-[amino-(2,4,6-trichloroanilino)methylidene]-2-methylguanidine;hydrochloride

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

To 20 g (0.1 mole) of 2,4,6-trichloroaniline and 12.6 g (0.1 mole) of 1-methyl-3-cyanoguanidine in 10 ml (0.1 mole) of concentrated hydrochloric acid is added 125 ml of n-butanol. The reaction mixture is refluxed for 17 hours, cooled and the alcohol evaporated off. The residue is extracted with ether after making it alkaline with 40% sodium hydroxide. The ether extract is dried over potassium carbonate and evaporated. The residue is dissolved in methanol, the pH adjusted to about 7, charcoal filtered and evaporated. The residue is triturated with ether and the solid that forms is recrystallized from water to obtain 1-(2,4,6-trichlorophenyl)-5-methylbiguanide hydrochloride.

後処理

  1. temperatureThe reaction mixture is refluxed for 17 hours
  2. temperaturecooled
  3. customthe alcohol evaporated off
  4. extractionThe residue is extracted with ether
  5. extractionThe ether extract
  6. dry with materialis dried over potassium carbonate
  7. customevaporated
  8. dissolutionThe residue is dissolved in methanol
  9. filtrationfiltered
  10. customevaporated
  11. customThe residue is triturated with ether
  12. customthe solid that forms is recrystallized from water

出典と根拠

ORDレコード
ord-e5830e06368146c2b98d0d78dd43429d
出典データセット
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03996232

反応ノート

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