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

HRID 342039

반응식

HRID 342039 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 110192531-(1-Amino-1-cyanomethyl)-1-ethoxycarbonylcyclopropane수율 97%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f3cbe3dd6abe450fa034e3267b377377
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05856518

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