Ethylene Glycol → HCID 20294078, 화합물

HRID 262435노트

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HRID 262435 반응식
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]

참가 물질

7

반응물 5

HCID 174Ethylene GlycolHCID 7860GlyoxalHCID 14797Potassium Hydroxide3회HCID 3051422-[2-(Cyanomethyl)-4,5-dimethylphenyl]acetonitrileHCID 21880647Glyoxal hydrate

생성물 1

HCID 20294078HCID 20294078, 화합물수율 31%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-30065f9e5db74ae8a3ea7f20249c7df4
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04154754

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