Ethyl cyanoacetate → Ethyl 1-cyanocyclopropanecarboxylate

HRID 1485048

反応式

HRID 1485048 の反応式
[C:1]([CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5])#[N:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:16][CH2:17]Br>CC(C)=O>[C:1]([C:3]1([C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH2:17][CH2:16]1)#[N:2]

参加物

5

反応物 3

HCID 7764Ethyl cyanoacetateHCID 78391,2-DibromoethaneHCID 11430Potassium Carbonate

生成物 1

HCID 380810Ethyl 1-cyanocyclopropanecarboxylate収率 97.8%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of ethyl cyanoacetate (11.8 g) in acetone (83.0 mL), potassium carbonate (43.1 g) and 1,2-dibromoethane (39.2 g) were added and the mixture was refluxed for 12 hours. After being cooled to room temperature, the reaction mixture was filtered through Celite (registered trademark). The filtrate was concentrated under reduced pressure and further dried under reduced pressure with heating to give ethyl 1-cyanocyclopropanecarboxylate as a red oil (14.2 g).

後処理

  1. temperaturethe mixture was refluxed for 12 hours
  2. filtrationthe reaction mixture was filtered through Celite (registered trademark)
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customfurther dried under reduced pressure
  5. temperaturewith heating

出典と根拠

ORDレコード
ord-650f3f851e6e4dbd963a263cf0dcaa28
出典データセット
uspto-grants-2016_08
特許番号
US09422240B2

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