Hydrochloric Acid → trans-Aconitic acid

HRID 904908

반응식

HRID 904908 반응식
[OH-].[Ca+2].[OH-].Cl.[C:5]([OH:17])(=[O:16])[CH:6]([CH:8]([CH2:12][C:13]([OH:15])=[O:14])[C:9]([OH:11])=[O:10])O>O>[CH2:12]([C:13]([OH:15])=[O:14])/[C:8](/[C:9]([OH:11])=[O:10])=[CH:6]\[C:5]([OH:17])=[O:16]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 1198Isocitric AcidHCID 6093208Calcium Hydroxide2회

생성물 1

HCID 444212trans-Aconitic acid수율 60%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
75 °C

실험 절차

Thirty one grams (0.1 mole) of product prepared as in Example I-B is mixed with 200 mls water. Thirty grams (0.4 mole) calcium hydroxide is added slowly while the pH of the reaction medium is maintained at 10-10.5 and the temperature is kept between 70° and 75° C. After the addition of calcium hydroxide is complete, the reaction mixture is stirred at 75° C. for an additional two hours and then cooled. 90 grams of a 20% by weight hydrochloric acid solution is added slowly to a pH of 1.3 and the resulting solution is then filtered. The filtrate is evaporated to dryness in vacuo and the residue extracted with acetone. The acetone extract is filtered and 19.5 grams of product consisting of 53.5% (60% yield) transaconitic acid and 5.8% of a mixture of lactones of isocitric acid and alloisocitric acid.

후처리

  1. temperatureis maintained at 10-10.5
  2. customis kept between 70° and 75° C
  3. temperaturecooled
  4. filtrationthe resulting solution is then filtered
  5. customThe filtrate is evaporated to dryness in vacuo
  6. extractionthe residue extracted with acetone
  7. extractionThe acetone extract
  8. filtrationis filtered

출처 및 근거

ORD 기록
ord-08434ff1ebe44b05a3d415375d40b38a
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04420621

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