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Methyl iodide → 1,3,5-Triazino(1,2-a)benzimidazol-4(3H)-one, 2,10-dihydro-2,2,3,10-tetramethyl-

HRID 615293
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HRID 615293 반응식
[CH3:1][C:2]1([CH3:17])[N:10]([CH3:11])[C:9](=[O:12])[N:8]2[C:4](=[N:5][C:6]3[CH:16]=[CH:15][CH:14]=[CH:13][C:7]=32)[NH:3]1.CI.[C:20](=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:1][C:2]1([CH3:17])[N:10]([CH3:11])[C:9](=[O:12])[N:8]2[C:4]([N:5]([CH3:20])[C:6]3[CH:16]=[CH:15][CH:14]=[CH:13][C:7]=32)=[N:3]1
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참가 물질

5

반응물 3

HCID 6328Methyl iodide2회HCID 11430Potassium CarbonateHCID 1591201,2-dihydro-2,2,3-trimethyl-1,3,5-triazino[1,2-a]benzimidazol-4(3H)-one

생성물 1

HCID 1591111,3,5-Triazino(1,2-a)benzimidazol-4(3H)-one, 2,10-dihydro-2,2,3,10-tetramethyl-수율 101.8%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 2.0 g (0.0087 mole) 1,2-dihydro-2,2,3-trimethyl-1,3,5-triazino[1,2-a]benzimidazol-4(3H)-one, 1.1 ml (0.0174 mole) methyl iodide, anhydrous potassium carbonate (1 gram) and acetone (100 ml) was heated under reflux, with stirring, overnight. After refluxing had continued 21 hours an additional 1 ml of methyl iodide was added and solids removed from the mixture by suction filtration. The filtrate was evaporated under reduced pressure and the resulting residue dissolved in ethyl acetate, washed with water, then with brine and dried over MgSO4, filtered and solvent stripped off to give B 1.8 g of crude product. Purification by high pressure liquid chromatography gave a solid, mp 79°-82° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux
  3. temperatureAfter refluxing
  4. waithad continued 21 hours
  5. customsolids removed from the mixture by suction filtration
  6. customThe filtrate was evaporated under reduced pressure
  7. dissolutionthe resulting residue dissolved in ethyl acetate
  8. washwashed with water
  9. dry with materialwith brine and dried over MgSO4
  10. filtrationfiltered

출처 및 근거

ORD 기록
ord-7c234314c36d491eb8ff3be0150a7f62
출처 데이터셋
uspto-grants-1985_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04498920

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