Sodium Chloride → Ethyl 2-amino-2-cyanoacetate

HRID 73601

反応式

HRID 73601 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 288716Ethyl 2-amino-2-cyanoacetate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-104f0b7a1d864791bee83ff07934004f
出典データセット
uspto-grants-2014_09
特許番号
US08829193B2

関連ノート

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