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Benzaldehyde → 2-Cyano-3-phenylprop-2-enoic acid

HRID 225155
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HRID 225155 반응식
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:9]([CH2:11][C:12]([O:14]C(C)C)=[O:13])#[N:10].N1CCCCC1>C(O)(=O)C>[C:9]([C:11](=[CH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:12]([OH:14])=[O:13])#[N:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 240BenzaldehydeHCID 8082PiperidineHCID 25917Isopropyl cyanoacetate

생성물 1

HCID 705342-Cyano-3-phenylprop-2-enoic acid

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 95 g of benzaldehyde, 114.3 g of 7A, 1 g of piperidine and 200 ml of acetic acid was heated on a steam bath for 1 hour. The acetic acid and unreacted benzaldehyde were distilled off, to 100° C./0.2 Torr. The residue was extracted with hot hexane; no residue was left. The solution was chilled, and the solid that formed was recrystallized from methanol to give the 1-methylethyl ester of 2-cyano-3-phenyl-2-propenoic acid (7B), mp: 72°-73° C.

후처리

  1. temperaturewas heated on a steam bath for 1 hour
  2. distillationThe acetic acid and unreacted benzaldehyde were distilled off, to 100° C./0.2 Torr
  3. extractionThe residue was extracted with hot hexane
  4. waitno residue was left
  5. temperatureThe solution was chilled
  6. customthe solid that formed
  7. customwas recrystallized from methanol

출처 및 근거

ORD 기록
ord-8db14a2049184cc49281b1470652e865
출처 데이터셋
uspto-grants-1980_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04235923

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