Acetic Acid → Methyl 4-cyanobenzenecarboximidate

HRID 1588571

반응식

HRID 1588571 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]#[N:10])=[CH:5][CH:4]=1)#[N:2].C[O-].[Na+].[C:14](O)(=[O:16])C>CO>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9](=[NH:10])[O:16][CH3:14])=[CH:5][CH:4]=1)#[N:2]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 121721,4-DicyanobenzeneHCID 10942334Sodium Methoxide

생성물 1

HCID 19734579Methyl 4-cyanobenzenecarboximidate수율 706.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1,4-dicyanobenzene (6.41 g, 50 mmol) was suspended in methanol (100 ml), and sodium methoxide (0.27 g, 5.0 mmol) was added. The mixture was stirred at room temperature for 22 hours. After the reaction was completed, acetic acid (0.31 g, 5.1 mmol) was added to neutralize the reaction solution, and the solution was concentrated under reduced pressure. Dichloromethane (50 ml) and diethyl ether (50 ml) were added to the concentrated residue, and insolubles were removed by filtration. The filtrate was concentrated under reduced pressure to give the crude product of methyl 4-cyanobenzenecarboximidate (5.77 g) as colorless powder.

후처리

  1. concentrationthe solution was concentrated under reduced pressure
  2. additionDichloromethane (50 ml) and diethyl ether (50 ml) were added to the concentrated residue, and insolubles
  3. customwere removed by filtration
  4. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-600dc1fb03824929a6db2be2fae9990c
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05223508

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