Sodium Bicarbonate → 1-(4-Methoxybenzyl)-5-bromo-4-methyl-3-amino-2-pyridone

HRID 1005404ノート

反応式

HRID 1005404 の反応式
[CH3:1][O:2][C:3]1[CH:21]=[CH:20][C:6]([CH2:7][N:8]2[CH:13]=[C:12]([Br:14])[C:11]([CH3:15])=[C:10]([N+:16]([O-])=O)[C:9]2=[O:19])=[CH:5][CH:4]=1.C([O-])(O)=O.[Na+]>C(O)(=O)C.Cl.O>[CH3:1][O:2][C:3]1[CH:21]=[CH:20][C:6]([CH2:7][N:8]2[CH:13]=[C:12]([Br:14])[C:11]([CH3:15])=[C:10]([NH2:16])[C:9]2=[O:19])=[CH:5][CH:4]=1

参加物

6

反応物 2

HCID 516892Sodium BicarbonateHCID 217064791-(4-Methoxybenzyl)-5-bromo-4-methyl-3-nitro-2-pyridone

生成物 1

HCID 217064931-(4-Methoxybenzyl)-5-bromo-4-methyl-3-amino-2-pyridone収率 61.5%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

To a stirred solution of 1-(4-methoxybenzyl)-5-bromo-4-methyl-3-nitro-2-pyridone (0.23 g, 0.65 mmol) in glacial acetic acid (3 mL) was added a solution of stannous chloride dihydrate (1.0 g) in concentrated HCl (2 mL). After 3.5 hours, the reaction mixture was diluted with water, neutralized with NaHCO3, and extracted with methylene chloride. The organic phase was dried, filtered, and evaporated to give 1-(4-methoxybenzyl)-5-bromo-4-methyl-3-amino-2-pyridone (0.13 g, 0.40 mmol, 61%).

後処理

  1. extractionextracted with methylene chloride
  2. customThe organic phase was dried
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-d50d134e267746858ac45471d8f700fe
出典データセット
uspto-grants-2000_04
特許番号
US06054470

反応ノート

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