Malonic Acid → HCID 735855, 화합물

HRID 1164473노트

반응식

HRID 1164473 반응식
[C:1]([OH:7])(=[O:6])[CH2:2][C:3](O)=O.[O:8]([C:15]1[CH:16]=[C:17]([CH:20]=[CH:21][CH:22]=1)C=O)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.N1CCCCC1>N1C=CC=CC=1>[O:8]([C:15]1[CH:16]=[C:17]([CH:20]=[CH:21][CH:22]=1)[CH:3]=[CH:2][C:1]([OH:7])=[O:6])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 867Malonic AcidHCID 8082PiperidineHCID 382843-Phenoxybenzaldehyde

생성물 1

HCID 735855HCID 735855, 화합물수율 95%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
25 °C

실험 절차

62.4 g of malonic acid are dissolved in 100 ml of pyridine. After termination of the exothermal reaction, 99 g of 3-phenoxybenzaldehyde and 5 g of piperidine are added, the batch is refluxed for 3 hours, cooled to 25° C. and poured onto ice/concentrated hydrochloric acid in order to wash out pyridine and piperidine, while the acid precipitates in the form of crystals. After drying, 113.7 g (95% of theory) of 3-phenoxycinnamic acid, m.p. 107°-109° C., are obtained. 18 g (0.15 mol) of thionyl chloride are added to a suspension of 24 g (0.1 mol) of 3-phenoxycinnamic acid in 100 ml of toluene, and stirred for 3 hours at 30° C. After removal of the solvent in vacuo, distillation is carried out. 24.6 g (95% of theory) of 3-(2-phenoxyphenyl)-2-propenic acid chloride, b.p. 155°-158° C./0.2 mm Hg, are obtained.

후처리

  1. additionare added
  2. temperaturethe batch is refluxed for 3 hours
  3. additionpoured onto ice/concentrated hydrochloric acid in order
  4. washto wash out pyridine and piperidine, while the acid
  5. customprecipitates in the form of crystals
  6. customAfter drying

출처 및 근거

ORD 기록
ord-cec9aaa58e4f44b1aa32fda69d35ea8f
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04370277

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