2-(Ethoxymethylene)propanedinitrile → HCID 18689500、化合物

HRID 1871872ノート

反応式

HRID 1871872 の反応式
[Cl:1][C:2]1[C:3]([NH:13][NH2:14])=[N:4][C:5]([Cl:12])=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.C(O[CH:18]=[C:19]([C:22]#[N:23])[C:20]#[N:21])C>C(O)C>[NH2:23][C:22]1[N:13]([C:3]2[C:2]([Cl:1])=[CH:7][C:6]([C:8]([F:10])([F:11])[F:9])=[C:5]([Cl:12])[N:4]=2)[N:14]=[CH:18][C:19]=1[C:20]#[N:21]

参加物

4

反応物 2

HCID 671522-(Ethoxymethylene)propanedinitrileHCID 110757282(1H)-Pyridinone, 3,6-dichloro-5-(trifluoromethyl)-, hydrazone

生成物 1

HCID 18689500HCID 18689500、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
20 °C

実験手順

24.6 g (0.1 mol) of 3,6-dichloro-2-hydrazino-5-trifluoromethylpyridine were added to a mixture of 12.2 g (0.1 mol) of ethoxymethylenemalononitrile and 200 ml of ethanol with stirring at 20° C. and it was stirred at 78° C. for 10 hours. After cooling, the reaction mixture was concentrated under reduced pressure and the residue was taken up in methylene chloride. It was extracted 3× with water and the organic phase separated off was dried over magnesium sulfate, filtered off with suction through neutral alumina and then concentrated under reduced pressure. After stirring in ether/pentane, 13.3 g (41.3% of theory) of the title compound of m.p. 168-171° C. were obtained (Active Compound Example No. 2a.002).

後処理

  1. stirringit was stirred at 78° C. for 10 hours
  2. temperatureAfter cooling
  3. concentrationthe reaction mixture was concentrated under reduced pressure
  4. extractionIt was extracted 3× with water
  5. customthe organic phase separated off
  6. dry with materialwas dried over magnesium sulfate
  7. filtrationfiltered off with suction through neutral alumina
  8. concentrationconcentrated under reduced pressure
  9. stirringAfter stirring in ether/pentane

出典と根拠

ORDレコード
ord-814137766be24e4eba8160aa1dd879d8
出典データセット
uspto-grants-2000_08
特許番号
US06107253

反応ノート

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