Ammonia → 1-(6-Methylpyridin-3-yl)-2-(4-(methylthio)phenyl)ethanone

HRID 413471ノート

反応式

HRID 413471 の反応式
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9](C#N)[C:10]([C:12]2[CH:13]=[N:14][C:15]([CH3:18])=[CH:16][CH:17]=2)=[O:11])=[CH:5][CH:4]=1.Cl.N>C(O)(=O)C>[CH3:1][S:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:9][C:10]([C:12]2[CH:13]=[N:14][C:15]([CH3:18])=[CH:16][CH:17]=2)=[O:11])=[CH:7][CH:8]=1

参加物

5

反応物 3

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 113005423-[2-(4-(Methylthio)phenyl)-2-cyanoacetyl](6-methyl)pyridine

生成物 1

HCID 101313251-(6-Methylpyridin-3-yl)-2-(4-(methylthio)phenyl)ethanone

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 8.0 g (28 mmol) of 3-[2-(4-(methylthio)phenyl)-2-cyanoacetyl](6-methyl)pyridine, 20 ml of acetic acid and 60 ml of concentrated hydrochloric acid was heated at 95° C. to 100° C. for 1.5 h. The orange solution was cooled and adjusted to pH 10 using concentrated ammonia solution. The resulting yellow-beige suspension was filtered and the residue was washed with water and dried. This gave 5.35 g (74%) of the title product in the form of a yellow solid.

後処理

  1. temperaturewas heated at 95° C. to 100° C. for 1.5 h
  2. temperatureThe orange solution was cooled
  3. filtrationThe resulting yellow-beige suspension was filtered
  4. washthe residue was washed with water
  5. customdried

出典と根拠

ORDレコード
ord-87f0bc21fb9f474f983355df71f91fd3
出典データセット
uspto-grants-2003_05
特許番号
US06566527B1

反応ノート

読み込み中…