Potassium Cyanide → 1-(1-Amino-1-cyanomethyl)-1-ethoxycarbonylcyclopropane

HRID 342039

反応式

HRID 342039 の反応式
[C-:1]#[N:2].[K+].[Cl-].[NH4+:5].O.N.[CH:8]([C:10]1([C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH2:12][CH2:11]1)=O>O.C(O)C>[NH2:5][CH:8]([C:10]1([C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH2:12][CH2:11]1)[C:1]#[N:2]

参加物

7

反応物 4

HCID 9032Potassium CyanideHCID 25517Ammonium ChlorideHCID 9964122Ethyl 1-formylcyclopropanecarboxylateHCID 12896473Azane;hydrate

生成物 1

HCID 110192531-(1-Amino-1-cyanomethyl)-1-ethoxycarbonylcyclopropane収率 97%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

An eggplant type flask was charged with 3.49 g of potassium cyanide and 3.74 g of ammonium chloride, and the contents were dissolved in 20 ml of water. After adding 40 ml of concentrated ammonia water to the solution, 5.01 g of ethyl 1-formylcyclopropane-1-carboxylate dissolved in 30 ml of ethanol was added thereto dropwise at room temperature, and the reaction solution was stirred for 2 hours at 50° C. After confirming completion of the reaction, the reaction solution was mixed with ice water and extracted with ethyl acetate. Next, the resulting organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and, after removing insoluble matter by filtration, concentrated under a reduced pressure. Thereafter, the resulting residue was subjected to a silica gel column chromatography (ethyl acetate) to obtain 5.44 g (97%) of the title compound in the form of colorless oil.

後処理

  1. additionwas added
  2. customcompletion of the reaction
  3. extractionextracted with ethyl acetate
  4. washNext, the resulting organic layer was washed with water and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customafter removing insoluble matter
  7. filtrationby filtration
  8. concentrationconcentrated under a reduced pressure

出典と根拠

ORDレコード
ord-f3cbe3dd6abe450fa034e3267b377377
出典データセット
uspto-grants-1999_01
特許番号
US05856518

関連ノート

読み込み中…