Ethyl 1-cyanocyclopropanecarboxylate → Ethyl 1-(aminomethyl)cyclopropanecarboxylate

HRID 1485049

반응식

HRID 1485049 반응식
[C:1]([C:3]1([C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH2:5][CH2:4]1)#[N:2].[H][H]>C(O)C.[Ni]>[NH2:2][CH2:1][C:3]1([C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH2:5][CH2:4]1

참가 물질

5

반응물 2

HCID 380810Ethyl 1-cyanocyclopropanecarboxylateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 11480505Ethyl 1-(aminomethyl)cyclopropanecarboxylate수율 93%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

반응 조건

온도
40 °C

실험 절차

To a solution in ethanol (127 mL) of the compound (14.0 g) obtained in step (1) above, a Raney nickel catalyst (about 2.8 g) was added. In a hydrogen atmosphere, the mixture was stirred at room temperature for 12 hours and further stirred at 40° C. for 12 hours. After being cooled to room temperature, the reaction mixture was filtered through Celite (registered trademark) and the filtrate was concentrated under reduced pressure. The resulting precipitate was recovered by filtration and washed with ethanol. The filtrate was concentrated to give the titled compound as a red oil (13.4 g).

후처리

  1. temperatureAfter being cooled to room temperature
  2. filtrationthe reaction mixture was filtered through Celite (registered trademark)
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. filtrationThe resulting precipitate was recovered by filtration
  5. washwashed with ethanol
  6. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-f579ef5bccaa4fd8991178f7c4ffeccc
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422240B2

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