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Pyridine → 4-(4-Fluorophenyl)-3-[(3,4-methylenedioxyphenyl)oxycarbonyl]-piperidine-6-one

HRID 2084610
ノート
印刷プレビュー

反応式

HRID 2084610 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][C:12](=[O:14])[NH:11][CH2:10][CH:9]2[CH2:15]CC(O)=O)=[CH:4][CH:3]=1.[OH-:20].[Na+].S(Cl)(Cl)=O.S(=O)=O.N1C=CC=CC=1.[CH2:35]1[O:39][C:38]2[CH:40]=[C:41]([OH:44])[CH:42]=[CH:43][C:37]=2[O:36]1>C(O)C.C(Cl)(Cl)Cl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:13][C:12](=[O:14])[NH:11][CH2:10][CH:9]2[C:15]([O:44][C:41]2[CH:42]=[CH:43][C:37]3[O:36][CH2:35][O:39][C:38]=3[CH:40]=2)=[O:20])=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 1049PyridineHCID 1119Sulfur DioxideHCID 14798Sodium HydroxideHCID 24386Thionyl ChlorideHCID 68289SesamolHCID 227338414-(4-Fluorophenyl)-3-carboxyethylpiperidin-6-one

生成物 1

HCID 22733847
4-(4-Fluorophenyl)-3-[(3,4-methylenedioxyphenyl)oxycarbonyl]-piperidine-6-one
収率 51.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 6212Chloroform溶媒

反応条件

温度
60 °C

実験手順

A solution of 4-(4-fluorophenyl)-3-carboxyethylpiperidin-6-one (0.5 g, 1.88 mmol, trans/cis ratio 56:44) in ethanol (10 ml) was added to a solution of sodium hydroxide (0.08 g, 2 mmol) in 95% ethanol (5 ml) and the mixture heated for 4 hours at 60° C. The solvent was removed at reduced pressure and the residue of water removed by distillation with toluene. The residue was suspended in dichloromethane (5 ml), treated with a solution of thionyl chloride (0.24 g, 2 mmol), and the mixture was brought to reflux. After 1 hour evolution of sulphur dioxide ceased, so the mixture was cooled to room temperature and treated with pyridine (0.16 g, 2 mmol) followed by a solution of sesamol (0.24 g, 1.75 mmol) in chloroform (2.5 ml). The resulting mixture was brought to reflux, heated for 4 hours, and stirred at ambient temperature for 2 days. The solvent was then removed at reduced pressure and the residue treated with water (5 ml), then extracted with ethyl acetate (20 and 10 ml). The organic extracts were combined, washed with brine (20 ml), dried over anhydrous sodium sulphate, filtered and evaporated to give the title compound (0.32 g).

後処理

  1. customThe solvent was removed at reduced pressure
  2. customthe residue of water removed by distillation with toluene
  3. temperatureto reflux
  4. temperaturewas cooled to room temperature
  5. temperatureto reflux
  6. temperatureheated for 4 hours
  7. customThe solvent was then removed at reduced pressure
  8. additionthe residue treated with water (5 ml)
  9. extractionextracted with ethyl acetate (20 and 10 ml)
  10. washwashed with brine (20 ml)
  11. dry with materialdried over anhydrous sodium sulphate
  12. filtrationfiltered
  13. customevaporated

出典と根拠

ORDレコード
ord-ca0b17549cdc40728873bf781931c97d
出典データセット
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06716985B2

反応ノート

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