Hydrochloric Acid → 2-(1-Pyrrolidinyl)-3-pyridinol

HRID 63393

Reaktionsgleichung

Reaktionsgleichung von HRID 63393
Br[C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[NH:9]1[CH2:13][CH2:12][CH2:11][CH2:10]1.Cl>>[N:9]1([C:2]2[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=2)[CH2:13][CH2:12][CH2:11][CH2:10]1

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 230702-Bromo-3-pyridinolHCID 31268Pyrrolidine

Produkt 1

HCID 900023802-(1-Pyrrolidinyl)-3-pyridinolAusbeute 41,3 %

Versuchsvorschrift

2-bromopyridin-3-ol (200 mg, 1.15 mmol) and pyrrolidine (184 mg, 2.58 mmol) were added in a reaction tube, followed by reacting in microwave at 120° C. for 20 minutes. The reaction mixture was added with 1 M HCl solution to neutralized, and extracted with ethyl acetate and dichloromethane. The obtained organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The concentrate was purified by column chromatography to obtain 2-(pyrrolidin-1-yl)pyridin-3-ol (78 mg, 41%).

Aufarbeitung

  1. extractionextracted with ethyl acetate and dichloromethane
  2. dry with materialThe obtained organic layer was dried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe concentrate was purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-48275c11308c4f8f9f29ea0f02a7e2d8
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09447083B2

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