Acetic Acid → HCID 178514356、化合物

HRID 2398036ノート

反応式

HRID 2398036 の反応式
CO[C:3](=[O:16])[C:4]1[C:9]([Cl:10])=[C:8]([Cl:11])[C:7]([Cl:12])=[C:6]([Cl:13])[C:5]=1[C:14]#[N:15].O.[NH2:18][NH2:19].C(O)(=O)C>CO>[Cl:13][C:6]1[C:7]([Cl:12])=[C:8]([Cl:11])[C:9]([Cl:10])=[C:4]2[C:5]=1[C:14](=[N:18][NH2:19])[NH:15][C:3]2=[O:16]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 79319Benzoic acid, 2,3,4,5-tetrachloro-6-cyano-, methyl ester

生成物 1

HCID 178514356HCID 178514356、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
10 °C

実験手順

119.6 g of 3,4,5,6-tetrachloro-2-cyanobenzoic acid methyl ester are dissolved in 600 ml of methanol and 70.6 g of a 30.6% strength methanolic solution of Na methylate. The solution is cooled to 10° C and is added dropwise at 10° C to a solution of 200 ml of hydrazine hydrate in 400 ml of methanol. A yellowish precipitate is formed. The reaction mixture is stirred at room temperature for 2 hours and is then warmed to 35° C over the course of 30 minutes and 200 ml of glacial acetic acid are added at this temperature. After stirring for 1 hour at room temperature, the product is filtered off and the filter residue is washed with methanol and water. The material filtered off is then extracted by boiling in 1 l of methylcellosolve for a further 2 hours, filtered off at room temperature and washed with methylcellosolve and methanol. After drying at 70° C, 98 g (82% of theory) of analytically pure 4,5,6,7-tetrachloro-isoindolin-1-on- 3-ylidene hydrazine of the formula ##STR31## are obtained.

後処理

  1. customA yellowish precipitate is formed
  2. additionare added at this temperature
  3. stirringAfter stirring for 1 hour at room temperature
  4. filtrationthe product is filtered off
  5. washthe filter residue is washed with methanol and water
  6. filtrationThe material filtered off
  7. extractionis then extracted
  8. waitby boiling in 1 l of methylcellosolve for a further 2 hours
  9. filtrationfiltered off at room temperature
  10. washwashed with methylcellosolve and methanol
  11. customAfter drying at 70° C

出典と根拠

ORDレコード
ord-34181bef555a4d9e8f47172bd2174b93
出典データセット
uspto-grants-1977_05
特許番号
US04024132

反応ノート

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