Imidazole → 2-(1-Imidazolyl)-4-dimethylamino-6-morpholino-1,3,5-triazine

HRID 2395610노트

반응식

HRID 2395610 반응식
Cl[C:2]1[N:7]=[C:6]([N:8]([CH3:10])[CH3:9])[N:5]=[C:4]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[N:3]=1.[OH-].[Na+].[NH:19]1[CH:23]=[CH:22][N:21]=[CH:20]1.ClCCl>CN(C=O)C.O>[N:19]1([C:2]2[N:7]=[C:6]([N:8]([CH3:10])[CH3:9])[N:5]=[C:4]([N:11]3[CH2:16][CH2:15][O:14][CH2:13][CH2:12]3)[N:3]=2)[CH:23]=[CH:22][N:21]=[CH:20]1

참가 물질

7

반응물 4

HCID 795ImidazoleHCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 105863421,3,5-Triazin-2-amine, 4-chloro-N,N-dimethyl-6-(4-morpholinyl)-

생성물 1

HCID 105643242-(1-Imidazolyl)-4-dimethylamino-6-morpholino-1,3,5-triazine수율 91.4%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

The obtained 2-chloro-4-dimethylamino-6-morpholino-1,3,5-triazine 492mg (2.02 mmol) was dissolved in DMF (20 ml), added with sodium hydroxide (182 mg, 4.55 mmol) and imidazole (308 mg, 4.52 mmol) and stirred at 110° C.-120° C. for 45 minutes. The reaction mixture was evaporated under reduced pressure. The residue obtained was added with dichloromethane and water, and then was shaken for mixing. The organic layer was separated from the mixture, washed with water and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and the residue was purified by silica gel column chromatography, using dichloromethane and methanol (95:5) as eluant, to obtain 508 mg (yield: 91.4%) of the titled compound as colorless crystals.

후처리

  1. customThe reaction mixture was evaporated under reduced pressure
  2. customThe residue obtained
  3. stirringwas shaken
  4. additionfor mixing
  5. customThe organic layer was separated from the mixture
  6. washwashed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe solvent was removed under reduced pressure
  9. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-ef8c3b85a43343ff9242c349ce1f5a3b
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05489591

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