Ethylene Glycol → HCID 20294078、化合物

HRID 262435ノート

反応式

HRID 262435 の反応式
C[C:2]1[C:7](C)=[CH:6][C:5]([CH2:9]C#N)=[C:4]([CH2:12]C#N)[CH:3]=1.[OH2:15].[CH:16]([CH:18]=[O:19])=O.[CH:20]([CH:22]=[O:23])=O.[OH-:24].[K+].[CH2:26](O)[CH2:27]O>CO>[CH3:9][C:5]1[CH:6]=[C:7]2[C:2](=[CH:3][C:4]=1[CH3:12])[C:20]([C:22]([OH:23])=[O:15])=[CH:27][CH:26]=[C:16]2[C:18]([OH:19])=[O:24]

参加物

7

反応物 5

HCID 174Ethylene GlycolHCID 7860GlyoxalHCID 14797Potassium Hydroxide3 回HCID 3051422-[2-(cyanomethyl)-4,5-dimethylphenyl]acetonitrileHCID 21880647Glyoxal hydrate

生成物 1

HCID 20294078HCID 20294078、化合物収率 31%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

18.4 parts of 4,5-dimethyl-1,2-bis-cyanomethyl-benzene and 8.4 parts of glyoxal hydrate (trimer) (3C2H2O2.2H2O), containing 80% of glyoxal to be liberated, are stirred in 100 parts by volume of methanol. With stirring and under nitrogen, 11.2 parts of powdered potassium hydroxide are added to the reaction mixture by small amounts at 0° to 5° C. After the addition of potassium hydroxide, stirring is continued for 5 hours at 0° to 5° C. under nitrogen. The slightly brown coloured reaction mixture is subsequently diluted with 100 parts by volume of ethylene glycol and then, after addition of 28 parts of potassium hydroxide, heated slowly to 190° C. under nitrogen while the methanol is distilled off and ammonia escapes at 80° C. After it has been stirred for 5 hours at 185° to 190° C. under nitrogen, the reaction mixture is worked up as described in Example 7 to yield 7.5 parts of 6,7-dimethyl-naphthalene-1,4-dicarboxylic acid (31% of theory) of formula ##STR52## in the form of slightly brown crystalline powder with a melting point of 268°-280° C.

後処理

  1. stirringstirring
  2. distillationis distilled off
  3. customat 80° C
  4. stirringAfter it has been stirred for 5 hours at 185° to 190° C. under nitrogen

出典と根拠

ORDレコード
ord-30065f9e5db74ae8a3ea7f20249c7df4
出典データセット
uspto-grants-1979_05
特許番号
US04154754

反応ノート

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