Methanol → 1,6-Dihydro-5(4H)-pyrimidinone O-methyloxime monohydrochloride

HRID 129815

反応式

HRID 129815 の反応式
O.[ClH:2].Cl.[NH2:4][CH2:5][C:6]([CH2:8][NH2:9])=O.[CH3:10][O:11][NH3+:12].[Cl-].[CH3:14]O>>[ClH:2].[CH3:10][O:11][N:12]=[C:6]1[CH2:8][NH:9][CH:14]=[N:4][CH2:5]1

参加物

4

反応物 3

HCID 887MethanolHCID 11639O-methylhydroxylammonium chlorideHCID 190837391,3-Diaminopropan-2-one--hydrogen chloride--water (1/2/1)

生成物 1

HCID 736056051,6-Dihydro-5(4H)-pyrimidinone O-methyloxime monohydrochloride収率 36%

実験手順

1,3-Diaminoacetone dihydrochloride monohydrate (2.61 g, 14.6 mmol) was dissolved in refluxing methanol. To this solution o-methylhydroxylamine hydrochloride (2.43 g, 29.2 mmol) was added. After reflexing for 48 hours the solvents were evaporated. The crude product was dissolved in methanol and an excess of trimethylorthoformate was added to the reaction mixture which was heated to reflux. After 24 hours the solvent was removed in vacuo. crystallization from methanol/ethyl acetate afforded 850 mg (36%) of a light-brown crystalline material. Mp. 170.7° C.

後処理

  1. customthe solvents were evaporated
  2. dissolutionThe crude product was dissolved in methanol
  3. additionan excess of trimethylorthoformate was added to the reaction mixture which
  4. temperaturewas heated to reflux
  5. customAfter 24 hours the solvent was removed in vacuo
  6. customcrystallization from methanol/ethyl acetate

出典と根拠

ORDレコード
ord-5a0b5e02eefc472db4304a28baf660fa
出典データセット
uspto-grants-1995_11
特許番号
US05470856

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