2,6-Dibromopyridine → 1-(6-Bromopyridin-2-yl)pyrrolidin-3-ol

HRID 385923

反応式

HRID 385923 の反応式
Br[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Br:8])[N:3]=1.[NH:9]1[CH2:13][CH2:12][CH:11]([OH:14])[CH2:10]1.CCCCCCC=CCCC>C1COCC1.C(OCC)(=O)C>[Br:8][C:4]1[N:3]=[C:2]([N:9]2[CH2:13][CH2:12][CH:11]([OH:14])[CH2:10]2)[CH:7]=[CH:6][CH:5]=1

参加物

6

実験手順

A mixture of 2,6-dibromopyridine (2.37 g, 0.01 mol), pyrrolidin-3-ol (1.0 g, 0.01 mol), 1,8-diazabicclo[5.4.0)-7-undecene (1.5 mL) in 10 mL of THF was heated at 70° C. under a nitrogen atmosphere for 11 hours. The reaction mixture was then cooled to room temperature, diluted with ethyl acetate (30 mL). The resulting solution was washed with water and brine, dried over anhydrous magnesium sulfate, filtered and concentrated. The residue was purified by silica gel chromatography (10-30% ethyl acetate/hexane) to give the title compound.

後処理

  1. washThe resulting solution was washed with water and brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel chromatography (10-30% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-23d8af70e5b34017a33c984f345e567d
出典データセット
uspto-grants-2013_02
特許番号
US08367706B2

関連ノート

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