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

HRID 2185125ノート

反応式

HRID 2185125 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

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).

後処理

  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.

出典と根拠

ORDレコード
ord-a1397595b60d41118d9c631c4a209fa4
出典データセット
uspto-grants-2002_06
特許番号
US06399781B1

反応ノート

読み込み中…