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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 615092
ノート
印刷プレビュー

反応式

HRID 615092 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6328Methyl iodide2 回HCID 11430Potassium CarbonateHCID 1591201,2-dihydro-2,2,3-trimethyl-1,3,5-triazino[1,2-a]benzimidazol-4(3H)-one

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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 1.8 g of crude product. Purification by high pressure liquid chromatography gave a solid, mp 79°-82° C.

後処理

  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

出典と根拠

ORDレコード
ord-3cd249cd169e49d49b0953154bdab7d9
出典データセット
uspto-grants-1985_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04497650

反応ノート

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