ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Ethylenediamine → N,N'''-Ethylenebis(1,3,5-triazine-2,4,6-triamine)

HRID 486378
ノート
印刷プレビュー

反応式

HRID 486378 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4](Cl)[N:3]=1.[CH2:10]([NH2:13])[CH2:11][NH2:12].[OH-].[Na+]>O>[CH2:10]([NH:13][C:4]1[N:3]=[C:2]([NH2:1])[N:7]=[C:6]([NH2:8])[N:5]=1)[CH2:11][NH:12][C:4]1[N:3]=[C:2]([NH2:1])[N:7]=[C:6]([NH2:8])[N:5]=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 3301EthylenediamineHCID 14798Sodium Hydroxide2 回HCID 188311,3,5-Triazine-2,4-diamine, 6-chloro-

生成物 1

HCID 6451884N,N'''-Ethylenebis(1,3,5-triazine-2,4,6-triamine)収率 91.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

29.1 g of 2,4-diamino-6-chloro-s-triazine was added to 300 ml of water to obtain a slurry. Then 6 g of ethylenediamine was added thereto, and the mixture was stirred for 15 minutes. Then, 16 g of a 25 wt% sodium hydroxide aqueous solution was added thereto, and the mixture was refluxed under heating for two hours. At that time, about 3 g of a 25 wt% sodium hydroxide aqueous solution was further gradually added over a period of two hours to maintain the reaction solution in a weakly alkaline state. After completion of the reaction, the reaction mixture was left to cool, whereupon the crystals were collected by filtration and washed with water to obtain 25.3 g of ethylenebismelamine. Then, 5.9 g of ethylenebismelamine and 17 g of formaline were mixed, and mixture was subjected to a heating reaction at 90° C. for 4 hours while maintaining the mixture at pH 9 to 10 with an aqueous sodium hydroxide solution. Then, the formed methylol product was taken out, and 30 ml of methanol was added thereto. The mixture was adjusted to pH 4 with hydrochloric acid. After the solution became uniform, it was heated for 5 minutes and neutralized. Then, methanol was distilled off to obtain 3.2 g of methoxymethylated ethylenebismelamine. The product was analyzed by IR and NMR and was found to be a mixture containing octamethoxymethylethylenebismelamine as the main component.

後処理

  1. customto obtain a slurry
  2. temperaturethe mixture was refluxed
  3. temperatureunder heating for two hours
  4. temperatureto maintain the reaction solution in a weakly alkaline state
  5. customAfter completion of the reaction
  6. waitthe reaction mixture was left
  7. temperatureto cool, whereupon the crystals
  8. filtrationwere collected by filtration
  9. washwashed with water

出典と根拠

ORDレコード
ord-ef596feca9b14529a35f4f472157e6ed
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05292614

反応ノート

読み込み中…

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