Sodium Chloride → Ethyl 2-amino-2-cyanoacetate

HRID 73601

반응식

HRID 73601 반응식
[C:1]([C:3](=[N:9]O)[C:4]([O:6][CH2:7][CH3:8])=[O:5])#[N:2].[O-]S(S([O-])=O)=O.[Na+].[Na+].[Cl-].[Na+]>O.C(=O)(O)[O-].[Na+]>[NH2:9][CH:3]([C:1]#[N:2])[C:4]([O:6][CH2:7][CH3:8])=[O:5]

참가 물질

6

반응물 3

HCID 5234Sodium ChlorideHCID 24489Sodium DithioniteHCID 6399078Ethyl 2-cyano-2-(hydroxyimino)acetate

생성물 1

HCID 288716Ethyl 2-amino-2-cyanoacetate

시약·촉매·용매 2

HCID 962Water용매HCID 516892Sodium Bicarbonate용매

실험 절차

To a solution of ethyl 2-cyano-2-(hydroxyimino)acetate (1 eq) in 70 mL of water and 56 mL of aq. sat. sodium bicarbonate was added portionwise throughout 10 minutes Na2S2O4 (2.8 eq) The reaction mixture was stirred at room temperature for 1 hour. The solution was saturated with sodium chloride, extracted with methylene chloride (300 mL×3) and then the combined organic layers were dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to give the titled compound, which was used to next step without further (55%). LC/MS (m/z): 129.0 (MH+), Rt:0.25 min.

후처리

  1. extractionextracted with methylene chloride (300 mL×3)
  2. dry with materialthe combined organic layers were dried over anhydrous Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-104f0b7a1d864791bee83ff07934004f
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829193B2

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