Hydrochloric Acid → HCID 54127586、化合物

HRID 2049033

反応式

HRID 2049033 の反応式
[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

参加物

9

反応物 6

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

生成物 1

HCID 54127586HCID 54127586、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 7914Diisopropyl Ether溶媒2 回

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-560419011467467dad868d28d2c8f93d
出典データセット
uspto-grants-1980_04
特許番号
US04196216

関連ノート

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