Potassium Carbonate → 4-(5-Bromo-pyridin-2-ylmethoxy)-1-[2-(4-hydroxymethyl-phenyl)-ethyl]-1H-pyridin-2-one

HRID 564141ノート

反応式

HRID 564141 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][N:5]([CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16][OH:17])=[CH:12][CH:11]=2)[C:4](=[O:18])[CH:3]=1.[Br:19][C:20]1[CH:21]=[CH:22][C:23]([CH2:26]Br)=[N:24][CH:25]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[Br:19][C:20]1[CH:21]=[CH:22][C:23]([CH2:26][O:1][C:2]2[CH:7]=[CH:6][N:5]([CH2:8][CH2:9][C:10]3[CH:15]=[CH:14][C:13]([CH2:16][OH:17])=[CH:12][CH:11]=3)[C:4](=[O:18])[CH:3]=2)=[N:24][CH:25]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 234380625-Bromo-2-(bromomethyl)pyridineHCID 580427304-Hydroxy-1-[2-(4-hydroxymethyl-phenyl)-ethyl]-1H-pyridin-2-one

生成物 1

HCID 670073734-(5-Bromo-pyridin-2-ylmethoxy)-1-[2-(4-hydroxymethyl-phenyl)-ethyl]-1H-pyridin-2-one

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To 1.23 g (5.00 mmol) 4-hydroxy-1-[2-(4-hydroxymethyl-phenyl)-ethyl]-1H-pyridin-2-one (preparation 2b) in 8.0 mL DMF is added 1.26 g (5.00 mmol) 5-bromo-2-bromomethyl-pyridine and 2.07 g (15.0 mmol) potassium carbonate. The reaction mixture is stirred overnight at RT, diluted with 80 mL of water, the formed precipitate is collected and dissolved in DMF. The solution is directly transferred to a reverse HPLC for purification (Zorbax stable bond, C18; water (0.15% formic acid)/acetonitrile 95:5 to 10:90).

後処理

  1. customthe formed precipitate is collected
  2. dissolutiondissolved in DMF
  3. customThe solution is directly transferred to a reverse HPLC for purification (Zorbax stable bond, C18; water (0.15% formic acid)/acetonitrile 95:5 to 10:90)

出典と根拠

ORDレコード
ord-20d0fa2894644f67b18eb9b4cc89c6d4
出典データセット
uspto-grants-2011_11
特許番号
US08067590B2

反応ノート

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