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

HRID 1485049

反応式

HRID 1485049 の反応式
[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

参加物

5

反応物 2

HCID 380810Ethyl 1-cyanocyclopropanecarboxylateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 11480505Ethyl 1-(aminomethyl)cyclopropanecarboxylate収率 93%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f579ef5bccaa4fd8991178f7c4ffeccc
出典データセット
uspto-grants-2016_08
特許番号
US09422240B2

関連ノート

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