Hydrochloric Acid → HCID 54127586, 화합물

HRID 2049033

반응식

HRID 2049033 반응식
[CH3:1][C:2](=[N:10][O:11][CH2:12][C:13]#N)[C:3]1[CH:8]=[CH:7][C:6]([Cl:9])=[CH:5][CH:4]=1.[Na].ClC1C=CC(C(=N[OH:26])C)=CC=1.ClCC#N.Cl.CN(C)[CH:34]=[O:35]>C(OC(C)C)(C)C.CO>[CH3:34][O:35][C:13](=[O:26])[CH2:12][O:11][N:10]=[C:2]([CH3:1])[C:3]1[CH:8]=[CH:7][C:6]([Cl:9])=[CH:5][CH:4]=1

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 7856ChloroacetonitrileHCID 96172p-Chloroacetophenone oximeHCID 5360545SodiumHCID 54535538(alpha-Methyl-4-chlorobenzylidene amino)oxy acetonitrile

생성물 1

HCID 54127586HCID 54127586, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 7914Diisopropyl Ether용매2회

실험 절차

Of the (α-methyl-4-chlorobenzylidene amino)oxy acetonitrile (melting point 57° C.-58.5° C.) which was obtained by reacting the sodium salt of 4'-chloroacetophenone oxime, with chloroacetonitrile in dimethylformamide, an amount of 11.3 g was dissolved in diisopropyl ether in which 1.94 g of hydrogen chloride and 1.73 g of methanol had also been dissolved. The solution was diluted with 25 ml of diisopropyl ether and subsequently stirred over night. Then the precipitate was drawn off, washed with absolute ether and dried in a vacuum. The resulting hydrochloride of methyl (α-methyl-4-chlorobenzylidene amino)oxy acetimidate melted at 95° C. with decomposition. After this substance had been dissolved in water, the superscribed ester separated out from the solution. It was extracted with ether and distilled in a vacuum. Boiling point at a pressure of 0.1 mm: 130° C.-132° C.

후처리

  1. dissolutionhad also been dissolved
  2. washwashed with absolute ether
  3. customdried in a vacuum
  4. dissolutionAfter this substance had been dissolved in water
  5. customthe superscribed ester separated out from the solution
  6. extractionIt was extracted with ether
  7. distillationdistilled in a vacuum
  8. custom130° C.-132° C.

출처 및 근거

ORD 기록
ord-560419011467467dad868d28d2c8f93d
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04196216

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