Bromine → 5-(Benzyloxy)-3-bromopyridin-2-amine

HRID 2277252ノート

反応式

HRID 2277252 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([NH2:15])=[N:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Br:16]Br.C(=O)([O-])O.[Na+]>C(O)(=O)C>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([Br:16])[C:12]([NH2:15])=[N:13][CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 24408BromineHCID 516892Sodium BicarbonateHCID 223152765-(Benzyloxy)pyridin-2-amine

生成物 1

HCID 582090735-(Benzyloxy)-3-bromopyridin-2-amine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 5-(benzyloxy)pyridin-2-amine (10.2 g) in acetic acid (50 mL) was added bromine (2.61 mL) at 0° C., and the mixture was stirred for 2 hr. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The obtained organic layer was dried over anhydrous magnesium sulfate, the solvent was evaporated, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (8.50 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe obtained organic layer was dried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated
  4. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-aa492df8b50740169374dbc757993210
出典データセット
uspto-grants-2015_09
特許番号
US09133129B2

反応ノート

読み込み中…