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Nitromethane → HCID 55250532, 화합물

HRID 1963074
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HRID 1963074 반응식
[F:1][C:2]1[C:3]([CH3:10])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=O.[N+:11]([CH3:14])([O-:13])=[O:12].C([O-])(=O)C.[NH4+]>C(O)(=O)C>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:4](/[CH:5]=[CH:14]/[N+:11]([O-:13])=[O:12])[C:3]=1[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6375NitromethaneHCID 517165Ammonium AcetateHCID 27792353-Fluoro-2-methylbenzaldehyde

생성물 1

HCID 55250532HCID 55250532, 화합물수율 89%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A Knoevenagel condensation was carried out by stirring 3-fluoro-2-methyl-benzaldehyde (20.721 g, 150 mmol), nitromethane (48.75 ml, 900 mmol) and ammonium acetate (34.687 g, 450 mmol) in 300 ml of acetic acid at 115° C. for 3.5 h. The mixture was evaporated to dryness under reduced pressure and the residue was dissolved in 250 ml of EA. The solution was washed with water (250 ml), three times with a 1 N sodium hydroxide solution (125 ml) and with brine (125 ml), dried over magnesium sulfate, filtered and evaporated to dryness. 24.18 g of the title compound were obtained as a yellow solid.

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후처리

  1. customA Knoevenagel condensation
  2. customThe mixture was evaporated to dryness under reduced pressure
  3. dissolutionthe residue was dissolved in 250 ml of EA
  4. washThe solution was washed with water (250 ml), three times with a 1 N sodium hydroxide solution (125 ml) and with brine (125 ml)
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-f5896acb88f6439195860fde8793f111
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415336B2

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