3-Phenylprop-2-enenitrile → Cinnamimidamide

HRID 2233212노트

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HRID 2233212 반응식
[C:1](#[N:10])[CH:2]=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[NH3:11].CO>CCO>[C:4]1(/[CH:3]=[CH:2]/[C:1](=[NH:11])[NH2:10])[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

4

반응물 2

HCID 746673-Phenylprop-2-enenitrileHCID 21705897Ammonia methanol

생성물 1

HCID 14668188Cinnamimidamide

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
0 °C

실험 절차

Cinnamonitrile (25.0 g, 194 mmol) was dissolved in EtOH (ethanol) (200 mL). The solution was cooled to 0° C. and HCl gas bubbled through the solution for 30 minutes. The solution was stirred at ambient temperature for 16 h and then concentrated under vacuum. The residue was dissolved in EtOH (100 mL), cooled to 0° C. and a solution of NH3/MeOH (7M, 69 mL, 484 mmol) was added dropwise through an addition funnel. Once added, the solution was allowed to warm to ambient temperature and the resulting NH4Cl was filtered off. The solution was concentrated under vacuum and the resulting white solid was used without further purification (26 g crude).

후처리

  1. customHCl gas bubbled through the solution for 30 minutes
  2. concentrationconcentrated under vacuum
  3. dissolutionThe residue was dissolved in EtOH (100 mL)
  4. temperaturecooled to 0° C.
  5. additionOnce added
  6. temperatureto warm to ambient temperature
  7. filtrationthe resulting NH4Cl was filtered off
  8. concentrationThe solution was concentrated under vacuum
  9. customthe resulting white solid was used without further purification (26 g crude)

출처 및 근거

ORD 기록
ord-32928aa9dc1446bfab1a8ab258d9abbc
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709483B2

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