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

HRID 129820

반응식

HRID 129820 반응식
O.[ClH:2].Cl.[NH2:4][CH2:5][C:6]([CH2:8][NH2:9])=O.Cl.[C:11]1([CH2:17][O:18][NH2:19])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[CH3:20]O>>[ClH:2].[C:11]1([CH2:17][O:18][N:19]=[C:6]2[CH2:8][NH:9][CH:20]=[N:4][CH2:5]2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 102312Benzyloxyamine hydrochlorideHCID 190837391,3-Diaminopropan-2-one--hydrogen chloride--water (1/2/1)

생성물 1

HCID 736056261,6-Dihydro-5(4H)-pyrimidinone O-(phenylmethyl)oxime monohydrochloride수율 60%

실험 절차

1,3-Diaminoacetone dihydrochloride monohydrate (2.00 g, 11.2 mmol) was dissolved in refluxing methanol and O-phenylmethylhydroxylamine hydrochloride (3.30 g, 20.5 mmol) was added. After refluxing for 20 hours the solvent was 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 48 hours the solvent was removed in vacuo. Crystallization from methanol/ethyl acetate afforded 1.60 g (60%) of white material. Mp. 167.5° C.

후처리

  1. additionwas added
  2. temperatureAfter refluxing for 20 hours the solvent
  3. customwas evaporated
  4. dissolutionThe crude product was dissolved in methanol
  5. additionan excess of trimethylorthoformate was added to the reaction mixture which
  6. temperaturewas heated to reflux
  7. customAfter 48 hours the solvent was removed in vacuo
  8. customCrystallization from methanol/ethyl acetate

출처 및 근거

ORD 기록
ord-48bf23f6d68a4a0d9472c998f54b63b0
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05470856

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