Ethyl formate → Sodium (E)-2-cyano-2-[(methoxycarbonyl)(methyl)amino]ethenolate

HRID 346532ノート

反応式

HRID 346532 の反応式
C[O-].[Na+:3].[C:4]([CH2:6][N:7]([CH3:12])[C:8](=[O:11])[O:9][CH3:10])#[N:5].[CH:13](OCC)=[O:14]>O1CCCC1>[C:4](/[C:6](/[N:7]([C:8]([O:9][CH3:10])=[O:11])[CH3:12])=[CH:13]\[O-:14])#[N:5].[Na+:3]

参加物

5

反応物 3

HCID 8025Ethyl formateHCID 10942334Sodium MethoxideHCID 45087346Methyl cyanomethyl(methyl)carbamate

生成物 1

HCID 57469797Sodium (E)-2-cyano-2-[(methoxycarbonyl)(methyl)amino]ethenolate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

0.46 g (0.01 mmol) of sodium methoxide is added under argon to tetrahydrofuran (solution A). Then 1.00 g (0.01 mmol) of methyl cyanomethyl(methyl)carbamate from Example 9A is added to 1.73 g (0.02 mmol) of ethyl formate. Solution A is slowly added dropwise to this mixture. The mixture is stirred at RT overnight. The solvent is concentrated in vacuo in a rotary evaporator, and diethyl ether is added to the residue. The crystals which have separated out are filtered off with suction and dried under high vacuum.

後処理

  1. concentrationThe solvent is concentrated in vacuo in a rotary evaporator, and diethyl ether
  2. additionis added to the residue
  3. customThe crystals which have separated out
  4. filtrationare filtered off with suction
  5. customdried under high vacuum

出典と根拠

ORDレコード
ord-78a196e817e64eb8ab1ec95dfae2af59
出典データセット
uspto-grants-2007_02
特許番号
US07173037B2

反応ノート

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