N,N'-Diallyl-6-chloro-1,3,5-triazine-2,4-diamine → 2,4-Bis-allylamino-6-[2-(2,2,6,6-tetramethylpiperid-4-yl)-ethylamino]-1,3,5-triazine

HRID 569194

反応式

HRID 569194 の反応式
[CH2:1]([NH:4][C:5]1[N:10]=[C:9]([NH:11][CH2:12][CH:13]=[CH2:14])[N:8]=[C:7](Cl)[N:6]=1)[CH:2]=[CH2:3].[CH3:16][C:17]1([CH3:28])[CH2:22][CH:21]([CH2:23][CH2:24][NH2:25])[CH2:20][C:19]([CH3:27])([CH3:26])[NH:18]1>C1(C)C(C)=CC=CC=1>[CH2:1]([NH:4][C:5]1[N:10]=[C:9]([NH:11][CH2:12][CH:13]=[CH2:14])[N:8]=[C:7]([NH:25][CH2:24][CH2:23][CH:21]2[CH2:22][C:17]([CH3:28])([CH3:16])[NH:18][C:19]([CH3:27])([CH3:26])[CH2:20]2)[N:6]=1)[CH:2]=[CH2:3]

参加物

4

反応物 2

HCID 27306N,N'-Diallyl-6-chloro-1,3,5-triazine-2,4-diamineHCID 125673674-Piperidineethanamine, 2,2,6,6-tetramethyl-

生成物 1

HCID 704152912,4-Bis-allylamino-6-[2-(2,2,6,6-tetramethylpiperid-4-yl)-ethylamino]-1,3,5-triazine

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

18.05 g (0.08 mole) of 2,4-bis-allylamino-6-chloro-1,3,5-triazine and 14.74 g (0.08 mole) of 2-(2,2,6,6-tetramethylpiperid-4-yl)-ethylamine in 130 ml of xylene are heated at reflux temperature for 4 hours, while stirring. 3.5 g (0.088 mole) of finely powdered sodium hydroxides are then added to the reaction mixture in 4 portions over a period of 4 hours, and the mixture is kept at reflux temperature overnight. The reaction mixture is then freed from the precipitated sodium chloride by filtration while hot, the xylene is completely removed by vacuum distillation, and the residue is recrystallised from n-pentane. The 2,4-bis-allylamino-6-[2-(2,2,6,6-tetramethylpiperid-4-yl)-ethylamino]-1,3,5-triazine thus obtained has a melting point of 74°-75° (stabiliser No. 14).

後処理

  1. temperatureat reflux temperature for 4 hours
  2. temperatureat reflux temperature overnight
  3. filtrationThe reaction mixture is then freed from the precipitated sodium chloride by filtration while hot, the xylene
  4. customis completely removed by vacuum distillation
  5. customthe residue is recrystallised from n-pentane

出典と根拠

ORDレコード
ord-803457f9cb924565ad9e82f8b0037346
出典データセット
uspto-grants-1988_03
特許番号
US04731393

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