Methanol → 1,6-Dihydro-5(4H)-pyrimidinone O-(2-propynyl)oxime monohydrochloride

HRID 129816

반응식

HRID 129816 반응식
O.[ClH:2].Cl.[NH2:4][CH2:5][C:6]([CH2:8][NH2:9])=O.Cl.[CH2:11]([O:14][NH2:15])[C:12]#[CH:13].[CH3:16]O>>[ClH:2].[CH2:11]([O:14][N:15]=[C:6]1[CH2:8][NH:9][CH:16]=[N:4][CH2:5]1)[C:12]#[CH:13]

참가 물질

4

반응물 3

HCID 887MethanolHCID 13502403O-(prop-2-yn-1-yl)hydroxylamine hydrochlorideHCID 190837391,3-Diaminopropan-2-one--hydrogen chloride--water (1/2/1)

생성물 1

HCID 736056041,6-Dihydro-5(4H)-pyrimidinone O-(2-propynyl)oxime monohydrochloride수율 36%

실험 절차

1,3-diaminoacetone dihydrochloride monohydrate (1.10 g, 6.14 mmol) was dissolved in refluxing methanol and O-(2-propynyl)hydroxylamine hydrochloride (0.730 g, 6.75 mmol) was added. After refluxing for 48 hours the solvent was evaporated. The crude product was dissolved in methanol and an excess of trimethylorthoformate was added to the reaction mixture and heated to reflux. After 24 hours the solvent was removed in vacuo. Crystallization from methanol/ethyl acetate afforded 410 mg (36%) of light-brown material. Mp. 205.0° C.

후처리

  1. additionwas added
  2. temperatureAfter refluxing for 48 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
  6. temperatureheated to reflux
  7. customAfter 24 hours the solvent was removed in vacuo
  8. customCrystallization from methanol/ethyl acetate

출처 및 근거

ORD 기록
ord-98086c9c03a94f4bbefe958470294dc0
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05470856

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