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

HRID 465453노트

반응식

HRID 465453 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7d261a97cc6a449e9da15e230b0d5ba5
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05153210

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