Water → 3-Methyl-isonicotinic acid

HRID 400164

反応式

HRID 400164 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([CH3:7])=[C:3]([CH3:8])[CH:2]=1.[Se](=O)=[O:10].[OH2:12]>C1(OC2C=CC=CC=2)C=CC=CC=1>[CH3:8][C:3]1[CH:2]=[N:1][CH:6]=[CH:5][C:4]=1[C:7]([OH:10])=[O:12]

参加物

5

反応物 3

HCID 962WaterHCID 114173,4-DimethylpyridineHCID 24007Selenium Dioxide

生成物 1

HCID 15020033-Methyl-isonicotinic acid収率 44%

試薬・触媒・溶媒 1

HCID 7583Diphenyl Ether溶媒

反応条件

温度
185 °C

実験手順

To a hot (155° C.) solution of 10.7 g (0.1 mol) of 3,4-lutidine in 100 mL diphenylether, was added 18 g (0.16 mol) selenium dioxide in portions. After about 20 minutes, the reaction was heated to 185° C. and allowed to react for approximately thirty minutes. After cooling, the reaction mixture was diluted with water and filtered. The filtrate was extracted with chloroform and the chloroform extracts were then concentrated under reduced pressure to provide 6.0 g of a pale brown solid.

後処理

  1. customto react for approximately thirty minutes
  2. temperatureAfter cooling
  3. filtrationfiltered
  4. extractionThe filtrate was extracted with chloroform
  5. concentrationthe chloroform extracts were then concentrated under reduced pressure

出典と根拠

ORDレコード
ord-879e9ee078d24867a087172f9db13fe0
出典データセット
uspto-grants-1998_10
特許番号
US05827858

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