Hydrochloric Acid → 4-[(3-Phenylprop-2-en-1-yl)oxy]piperidine

HRID 856062ノート

反応式

HRID 856062 の反応式
[C:1]1([CH:7]=[CH:8][CH2:9][O:10][CH:11]2[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[OH-].[Na+]>C(O)C>[C:1]1([CH:7]=[CH:8][CH2:9][O:10][CH:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 69479286Tert-butyl 4-(3-phenyl-2-propenyloxy)piperidine-1-carboxylate

生成物 1

HCID 537562574-[(3-Phenylprop-2-en-1-yl)oxy]piperidine収率 92.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

Tert-butyl 4-(3-phenyl-2-propenyloxy)-piperidine-1-carboxylate (0.314 g, 0.989 mmol) prepared in Reference Example 110 was dissolved in ethanol (10 ml), to which 6N hydrochloric acid aqueous solution (3 ml, 18 mmol) was added, and the mixture was stirred at 60° C. for 1 hour. The reaction mixture was neutralized with sodium hydroxide aqueous solution, and the mixture was extracted with methylene chloride. The extract was washed with brine, dried over sodium sulfate, and then filtered. The filtrate was concentrated under reduced pressure, and the residue was dried in vacuo to afford 4-(3-phenyl-2-propenyloxy)piperidine (0.198 g, yield 92%) as a yellow oil.

後処理

  1. additionwas added
  2. extractionthe mixture was extracted with methylene chloride
  3. washThe extract was washed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customthe residue was dried in vacuo

出典と根拠

ORDレコード
ord-4d88193233844b67b3496607afd68d08
出典データセット
uspto-grants-2007_08
特許番号
US07262212B2

反応ノート

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