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

HRID 856062노트

반응식

HRID 856062 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4d88193233844b67b3496607afd68d08
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262212B2

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