Allylamine → HCID 20148735, 화합물

HRID 569195노트

반응식

HRID 569195 반응식
[CH2:1]([NH2:4])[CH:2]=[CH2:3].[Cl:5][C:6]1[N:11]=[C:10](Cl)[N:9]=[C:8]([N:13]([CH:39]2[CH2:44][C:43]([CH3:46])([CH3:45])[NH:42][C:41]([CH3:48])([CH3:47])[CH2:40]2)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][N:20]([C:31]2[N:36]=[C:35]([Cl:37])[N:34]=[C:33](Cl)[N:32]=2)[CH:21]2[CH2:26][C:25]([CH3:28])([CH3:27])[NH:24][C:23]([CH3:30])([CH3:29])[CH2:22]2)[N:7]=1.[OH-].[Na+]>C1(C)C=CC=CC=1.O>[Cl:5][C:6]1[N:11]=[C:10]([NH:4][CH2:1][CH:2]=[CH2:3])[N:9]=[C:8]([N:13]([CH:39]2[CH2:40][C:41]([CH3:47])([CH3:48])[NH:42][C:43]([CH3:45])([CH3:46])[CH2:44]2)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][N:20]([C:31]2[N:36]=[C:35]([Cl:37])[N:34]=[C:33]([NH:4][CH2:1][CH:2]=[CH2:3])[N:32]=2)[CH:21]2[CH2:22][C:23]([CH3:29])([CH3:30])[NH:24][C:25]([CH3:28])([CH3:27])[CH2:26]2)[N:7]=1

참가 물질

6

반응물 3

HCID 7853AllylamineHCID 14798Sodium HydroxideHCID 21468019HCID 21468019, 화합물

생성물 1

HCID 20148735HCID 20148735, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

실험 절차

17.2 g (0.3 mole) of anhydrous allylamine are added dropwise, in the course of one hour, at 30°-40° and while stirring, to a solution of 103.6 g (0.15 mole) of N,N'-bis-(2,4-dichloro-1,3,5-triazin-6-yl)-N,N'-bis-(2,2,6,6-tetramethylpiperid-4-yl)-hexamethylenediamine in 500 ml of toluene. A solution of 12.0 g (0.3 mole) of sodium hydroxide in 100 ml of water is then added at approx. 30°, and stirring is continued for a further 19 hours at 50°. The mixture is worked up by separating off the aqueous phase in a separating funnel, washing the organic phase with three times 200 ml of water, drying it over sodium sulfate and removing the solvent by vacuum distillation. The solid residue is recrystallised from ethyl methyl ketone, which gives pure N,N'-bis-(2-chloro-4-allylamino-1,3,5-triazin-6-yl)-N,N'-bis-(2,2,6,6-tetramethylpiperid-4-yl)-hexamethylenediamine of melting point 210°-211°.

후처리

  1. customby separating off the aqueous phase in a separating funnel
  2. washwashing the organic phase with three times 200 ml of water
  3. dry with materialdrying it over sodium sulfate
  4. customremoving the solvent
  5. distillationby vacuum distillation
  6. customThe solid residue is recrystallised from ethyl methyl ketone, which

출처 및 근거

ORD 기록
ord-46754e814ff042cca44c5ee8b035efcf
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04731393

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