Sodium Acetate → Oxalic acid--4-(1-benzylpiperidin-3-yl)-1,2-phenylene diacetate (1/1)

HRID 2071416ノート

反応式

HRID 2071416 の反応式
[C:1]([O-:4])(=[O:3])[CH3:2].[Na+].[C:6]([OH:11])(=[O:10])[C:7]([OH:9])=[O:8].[CH2:12]([N:19]1[CH2:24][CH2:23][CH2:22][CH:21]([C:25]2[CH:30]=[CH:29][C:28](O)=[C:27]([OH:32])[CH:26]=2)[CH2:20]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(OC(=O)C)(=O)C>[C:6]([OH:11])(=[O:10])[C:7]([OH:9])=[O:8].[CH2:12]([N:19]1[CH2:24][CH2:23][CH2:22][CH:21]([C:25]2[CH:30]=[CH:29][C:28]([O:3][C:1](=[O:4])[CH3:2])=[C:27]([O:32][C:7](=[O:8])[CH3:6])[CH:26]=2)[CH2:20]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

4

反応物 2

HCID 517045Sodium AcetateHCID 20370845HCID 20370845、化合物

生成物 1

HCID 3046215Oxalic acid--4-(1-benzylpiperidin-3-yl)-1,2-phenylene diacetate (1/1)収率 224.9%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

反応条件

温度
20 °C

実験手順

9.8 g of anhydrous sodium acetate were added to a mixture of 9.8 g of the product of Step B and 120 ml of acetic acid anhydride and the mixture was stirred at 20° C. for 3 hours and was then filtered. The filter was washed with ethanol and the filtrate was evaporated to dryness under reduced pressure. The residue was taken up in water and ethyl acetate and the solution was made alkaline with an aqueous solution saturated with sodium bicarbonate. The ethyl acetate phase was recovered by decanting, was dried and evaporated to dryness. The residue was dissolved in 50 ml of isopropanol and a solution of 4 g of oxalic acid in 50 ml of isopropanol was added thereto. The mixture was refluxed until dissolution occurred and was cooled to 20° C. and vacuum filtered to obtain 13.5 g of N-benzyl-3-(3',4'-diacetoxyphenyl)-piperidine oxalate melting at 145° C.

後処理

  1. filtrationwas then filtered
  2. washThe filter was washed with ethanol
  3. customthe filtrate was evaporated to dryness under reduced pressure
  4. customThe ethyl acetate phase was recovered
  5. customby decanting
  6. customwas dried
  7. customevaporated to dryness
  8. dissolutionThe residue was dissolved in 50 ml of isopropanol
  9. additiona solution of 4 g of oxalic acid in 50 ml of isopropanol was added
  10. temperatureThe mixture was refluxed until dissolution
  11. temperaturewas cooled to 20° C.
  12. filtrationvacuum filtered

出典と根拠

ORDレコード
ord-e6122870b25a4837b16948fac292b706
出典データセット
uspto-grants-1977_09
特許番号
US04046901

反応ノート

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