Benzaldehyde → 2-(Methylsulanylmethyl)-3-phenylprop-2-enal

HRID 1448115

반응식

HRID 1448115 반응식
[OH-].[K+].[CH:3](=O)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH3:11][S:12][CH2:13][CH2:14][CH:15]=[O:16]>CO>[CH3:11][S:12][CH2:13][C:14](=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[CH:15]=[O:16]

참가 물질

5

반응물 3

HCID 240BenzaldehydeHCID 14797Potassium HydroxideHCID 18635Methional

생성물 1

HCID 533951952-(Methylsulanylmethyl)-3-phenylprop-2-enal수율 33.7%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Into a 100 ml three necked reaction flask equipped with stirrer, thermometer and addition funnel is charged a solution of 0.5 grams of potassium hydroxide in 10 ml methanol. Benzaldehyde (10.0 grams) is added as the mixture is cooled to 5°-10° C. Methional (10.0 grams) is then added dropwise while maintaining the reaction temperature at 5°-10° C. The mixture is then allowed to warm to room temperature and stirred for a period of 1 hour. Most of the solvent is evaporated at reduced pressure and the mixture is partitioned between water and ether. The organic layer is washed several times with water and once with saturated brine. The solvent is evaporated leaving a yellow oil which is distilled to give 6.1 grams product, boiling point 104°-111° C. (0.4 mm Hg).

후처리

  1. additionthermometer and addition funnel
  2. temperatureis cooled to 5°-10° C
  3. temperaturewhile maintaining the reaction temperature at 5°-10° C
  4. customMost of the solvent is evaporated at reduced pressure
  5. customthe mixture is partitioned between water and ether
  6. washThe organic layer is washed several times with water
  7. customThe solvent is evaporated
  8. customleaving a yellow oil which
  9. distillationis distilled

출처 및 근거

ORD 기록
ord-ce33db1961e748b9a25c110cc1812494
출처 데이터셋
uspto-grants-1979_12
특허 번호
US04179526

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