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

HRID 129815

반응식

HRID 129815 반응식
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

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5a0b5e02eefc472db4304a28baf660fa
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05470856

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