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

HRID 63393

反応式

HRID 63393 の反応式
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

参加物

4

反応物 3

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

生成物 1

HCID 900023802-(1-Pyrrolidinyl)-3-pyridinol収率 41.3%

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-48275c11308c4f8f9f29ea0f02a7e2d8
出典データセット
uspto-grants-2016_09
特許番号
US09447083B2

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