Sulfuric Acid → 4-Methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile

HRID 2185125노트

반응식

HRID 2185125 반응식
[C:1]([C:3]([C:10]#[N:11])=[C:4]([CH3:9])[CH:5]=[CH:6]OC)#[N:2].S(=O)(=O)(O)[OH:13]>O>[C:1]([C:3]1[C:10](=[O:13])[NH:11][CH:6]=[CH:5][C:4]=1[CH3:9])#[N:2]

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 725894471,1-Dicyano-4-methoxy-2-methyl-1,3-butadiene

생성물 1

HCID 106067824-Methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile수율 90.6%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

The mixture of 4,4-dicyano-3-methyl-3-butenal dimethyl acetatal (1) and 1, 1-dicyano-4-methoxy-2-methyl-1,3-butadiene (2) produced by the preceding step was added to a stirred solution of concentrated sulfuric acid (1 09.8 g, 1.12 moles) at a rate so that the reaction contents did not exceed 30° C. The reaction mixture was then heated to 50° C. and held at that temperature for 1.5 hours. The reaction mixture was cooled to ambient temperature followed by the addition of water (150 mL). The product was filtered from the reaction mixture, washed with water (20 mL) and dried in a vacuum oven at 70° C. and full vacuum for 12 hours to give 40.7 g of 3-cyano-4-methyl-2-pyridone (3).

후처리

  1. customproduced by the preceding step
  2. customdid not exceed 30° C
  3. temperatureThe reaction mixture was cooled to ambient temperature
  4. filtrationThe product was filtered from the reaction mixture
  5. washwashed with water (20 mL)
  6. customdried in a vacuum oven at 70° C.

출처 및 근거

ORD 기록
ord-a1397595b60d41118d9c631c4a209fa4
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06399781B1

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