Acetone → 5-Pyrimidinol, hexahydro-2,2-dimethyl-5-phenyl-

HRID 623203ノート

反応式

HRID 623203 の反応式
Cl.Cl.[OH:3][C:4]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([CH2:7][NH2:8])[CH2:5][NH2:6].[OH-].[Na+].[CH3:17][C:18]([CH3:20])=O>O>[CH3:17][C:18]1([CH3:20])[NH:8][CH2:7][C:4]([OH:3])([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:5][NH:6]1

参加物

5

反応物 3

HCID 180AcetoneHCID 14798Sodium HydroxideHCID 21290601HCID 21290601、化合物

生成物 1

HCID 30874705-Pyrimidinol, hexahydro-2,2-dimethyl-5-phenyl-収率 68.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

4.4 g (0.01841 mol) of the dihydrochloride obtained in stage (c) above are dissolved in 50 ml of water. 2.2 g of sodium hydroxide pellets and 3 ml of acetone are added. The mixture is left to stand overnight at room temperature (15°-20° C.) and extracted with 3×100 ml of CHCl3, and the chloroform phase is washed with 30 ml of water, dried over MgSO4 and then filtered to remove MgSO4. The filtrate is evaporated to dryness; recrystallization from petroleum ether (fraction boiling at 45°-60° C.) gives 2.6 g (yield: 68.5%) of CRL 41 365. M.p.=108° C.

後処理

  1. waitThe mixture is left
  2. extraction(15°-20° C.) and extracted with 3×100 ml of CHCl3
  3. washthe chloroform phase is washed with 30 ml of water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customto remove MgSO4
  7. customThe filtrate is evaporated to dryness
  8. customrecrystallization from petroleum ether (fraction boiling at 45°-60° C.)
  9. customgives 2.6 g (yield: 68.5%) of CRL 41 365

出典と根拠

ORDレコード
ord-3a4322d0a09041559f0772612c7e895d
出典データセット
uspto-grants-1988_09
特許番号
US04774248

反応ノート

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