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

반응식

HRID 569194 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-803457f9cb924565ad9e82f8b0037346
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04731393

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