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

HRID 346532노트

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HRID 346532 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-78a196e817e64eb8ab1ec95dfae2af59
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07173037B2

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