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Ethanol → HCID 86742227, 화합물

HRID 1590272
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HRID 1590272 반응식
[Cl-].[NH4+:2].[OH-].[NH4+].[CH3:5][O:6][N:7]=[C:8]([C:11]#[N:12])[C:9]#[N:10].[CH2:13]([OH:15])[CH3:14]>>[C:13]([O-:6])(=[O:15])[CH3:14].[C:9]([C:8](=[N:7][O:6][CH3:5])[C:11]([NH2:2])=[NH2+:12])#[N:10]
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참가 물질

5

반응물 4

HCID 702EthanolHCID 14923Ammonium HydroxideHCID 25517Ammonium ChlorideHCID 12474891Methoxyiminomalononitrile

생성물 1

HCID 86742227HCID 86742227, 화합물

실험 절차

To a mixed solution of ammonium chloride(14.2 g) dissolved in ethanol (90 ml) and conc. ammonium hydroxide aqueous solution (178 ml) was added 2-(methoxyimino)malononitrile(29 g) at -5°~0° C., and the mixture was stirred for 10 hours at these temperatures. The reaction mixture was extracted 3 times with methylene chloride (respectively, 450 ml, 100 ml and 100 ml), dehydrated, filtered, and concentrated. The residue was dissolved in ethyl acetate, and crystalized with acetic acid to give the above-indicated compound (20.5 g) in pale brown.

후처리

  1. extractionThe reaction mixture was extracted 3 times with methylene chloride (respectively, 450 ml, 100 ml and 100 ml),
  2. filtrationfiltered
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. customcrystalized with acetic acid

출처 및 근거

ORD 기록
ord-71cffb89e4f34f9d82b9a41ba55ce076
출처 데이터셋
uspto-grants-1993_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05202315

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