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Methylhydrazine → HCID 19917929, 화합물

HRID 1755872
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HRID 1755872 반응식
CNN.[OH:4][C:5]1[C:6](=[O:25])[N:7]([CH3:24])[C:8]([CH2:11][O:12][N:13]2C(=O)C3=CC=CC=C3C2=O)=[N:9][CH:10]=1>CN(C)C=O>[NH2:13][O:12][CH2:11][C:8]1[N:7]([CH3:24])[C:6](=[O:25])[C:5]([OH:4])=[CH:10][N:9]=1
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참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 19918009HCID 19918009, 화합물

생성물 1

HCID 19917929HCID 19917929, 화합물수율 73%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Methylhydrazine (92 mg) (2 mmol) are added at 0° C. to a suspension of 301 mg (1 mmol) of N-[(3,4-dihydro-5-hydroxy-3-methyl-4-oxo-2-pyrimidinyl)methoxy]phthalimide in 9 ml of absolute dimethylformamide. A solution gradually results and this is then stirred at room temperature for 3 hours. The solution is concentrated in a high vacuum at room temperature, the residue is washed with petroleum ether and finally 10 ml of water are added thereto. After good intermixing the mixture is filtered. The filtrate is concentrated, finally with toluene/ethanol. After crystallization from ethanol there are obtained 125 mg of 2-[(aminooxy)methyl]-5-hydroxy-3-methyl-4(3H)-pyrimidinone as white crystals of m.p. 106° C.

후처리

  1. customA solution gradually results
  2. concentrationThe solution is concentrated in a high vacuum at room temperature
  3. washthe residue is washed with petroleum ether and finally 10 ml of water
  4. additionare added
  5. filtrationAfter good intermixing the mixture is filtered
  6. concentrationThe filtrate is concentrated, finally with toluene/ethanol
  7. customAfter crystallization from ethanol

출처 및 근거

ORD 기록
ord-77713f4599d64438b87fa4278811e8bf
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05438052

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