Hydracrylonitrile → 2-Cyanoethyl prop-2-ynoate

HRID 67713

반응식

HRID 67713 반응식
[C:1]([OH:5])(=[O:4])[C:2]#[CH:3].[C:6](#[N:10])[CH2:7][CH2:8]O>C1(C)C=CC(S(O)(=O)=O)=CC=1.C(Cl)(Cl)Cl>[C:1]([O:5][CH2:8][CH2:7][C:6]#[N:10])(=[O:4])[C:2]#[CH:3]

참가 물질

5

반응물 2

HCID 8011HydracrylonitrileHCID 10110Propiolic Acid

생성물 1

HCID 204932242-Cyanoethyl prop-2-ynoate수율 29%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 6212Chloroform용매

실험 절차

A solution of 98 g of propiolic acid (1.4 moles), 99.5 g of hydracrylonitrile (1.4 moles), 2 g of p-toluenesulfonic acid and 200 ml of chloroform were refluxed, using a Soxhlet extractor filled with 3 A molecular sieves to remove the water generated during the esterification. A total reflux time of 94 hours was employed. The reaction was cooled, poured into water and extracted with chloroform. The combined extracts were washed with dilute bicarbonate solution, dried (MgSO4), and concentrated to give 49.2 g (29 percent) of a liquid used without purification.

후처리

  1. additionfilled with 3 A molecular sieves
  2. customto remove the water
  3. customA total reflux time of 94 hours
  4. temperatureThe reaction was cooled
  5. additionpoured into water
  6. extractionextracted with chloroform
  7. washThe combined extracts were washed with dilute bicarbonate solution
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4a87bb4296684e359b17c6a0c3e00635
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04346161

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