Hydrochloric Acid → Ethyl2-[4-(2-oxo-1-cyclohexylidenemethyl)phenyl]propionate

HRID 1902753노트

반응식

HRID 1902753 반응식
[CH:1]([C:3]1[CH:8]=[CH:7][C:6]([CH:9]([CH3:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:5][CH:4]=1)=O.N1([C:21]2[CH2:26][CH2:25][CH2:24][CH2:23][CH:22]=2)CCCC1.Cl.[OH2:28]>C1C=CC=CC=1>[O:28]=[C:21]1[CH2:26][CH2:25][CH2:24][CH2:23][C:22]1=[CH:1][C:3]1[CH:8]=[CH:7][C:6]([CH:9]([CH3:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:5][CH:4]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 707681-Pyrrolidino-1-cyclohexeneHCID 13066570rac 2-(4-Formylphenyl)propionic Acid Ethyl Ester

생성물 1

HCID 54259840Ethyl2-[4-(2-oxo-1-cyclohexylidenemethyl)phenyl]propionate

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

A mixture of 5.15 g of ethyl 2-(p-formylphenyl)propionate, 4.5 g of pyrrolidinocyclohexene and 20 ml of benzene was heated under reflux for 18 hours. After cooling, the reaction mixture was admixed with a mixture of 5 ml of conc. hydrochloric acid and 5 ml of water under ice-cooling and then stirred at room temperature overnight. 100 ml of benzene were added thereto, the organic layer was separated and then washed with water. After drying over anhydrous sodium sulfate, the benzene was distilled off to leave an oily substance. The substance was distilled under reduced pressure to afford 2.3 g of the desired product as a yellow oily substance having a boiling point of 160°-170° C./0.3 mmHg (bath temp.).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. temperatureAfter cooling
  4. temperaturecooling
  5. customthe organic layer was separated
  6. washwashed with water
  7. dry with materialAfter drying over anhydrous sodium sulfate
  8. distillationthe benzene was distilled off
  9. customto leave an oily substance
  10. distillationThe substance was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-b9f8d486d95b4204aa8d44b9ced88b30
출처 데이터셋
uspto-grants-1982_12
특허 번호
US04365076

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