Water → 3,4-dihydro-5-(4-acetonylphenyl)-6-methyl-2(1H)-pyridone

HRID 465453ノート

反応式

HRID 465453 の反応式
S(=O)(=O)(O)O.C1CO[C:8]([CH3:24])([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH:16]([C:21](=O)[CH3:22])[CH2:17][CH2:18][C:19]#[N:20])=[CH:12][CH:11]=2)[O:7]1.[OH2:27]>C(O)(=O)C>[CH2:9]([C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH2:17][CH2:18][C:19](=[O:27])[NH:20][C:21]=2[CH3:22])=[CH:12][CH:11]=1)[C:8]([CH3:24])=[O:7]

参加物

5

反応物 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 198745084-(4-(2,2-(Ethylenedioxy)propyl)phenyl)-5-oxo-hexane nitrile

生成物 1

HCID 198745593,4-dihydro-5-(4-acetonylphenyl)-6-methyl-2(1H)-pyridone

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Concentrated sulphuric acid (5 ml) was added dropwise to a solution of 4-(4-(2,2-(ethylenedioxy)propyl)phenyl)-5-oxo-hexane nitrile (3.09 g) in glacial acetic acid (21 ml). The orange solution was allowed to stand at room temperature for 3 days then poured into water and allowed to stand for 2 hr. The solution was extracted with chloroform, the organic layer separated, washed with sodium bicarbonate solution, dried (MgSO4) and evaporated to an oil (2.44 g) which was chromatographed on silica. Elution with chloroform gave 3,4-dihydro-5-(4-acetonylphenyl)-6-methyl-2(1H)-pyridone as an oil.

後処理

  1. waitto stand for 2 hr
  2. extractionThe solution was extracted with chloroform
  3. customthe organic layer separated
  4. washwashed with sodium bicarbonate solution
  5. dry with materialdried (MgSO4)
  6. customevaporated to an oil (2.44 g) which
  7. customwas chromatographed on silica
  8. washElution with chloroform

出典と根拠

ORDレコード
ord-7d261a97cc6a449e9da15e230b0d5ba5
出典データセット
uspto-grants-1992_10
特許番号
US05153210

反応ノート

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