Sulfuric Acid → Methyl 2-amino-6-chloronicotinate

HRID 77845ノート

反応式

HRID 77845 の反応式
S(=O)(=O)(O)O.[NH2:6][C:7]1[N:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:8]=1[C:9]([OH:11])=[O:10].[C:17](=O)([O-])O.[Na+]>CO>[CH3:17][O:10][C:9](=[O:11])[C:8]1[CH:12]=[CH:13][C:14]([Cl:16])=[N:15][C:7]=1[NH2:6]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 122639922-Amino-6-chloronicotinic acid

生成物 1

HCID 57415887Methyl 2-amino-6-chloronicotinate収率 68%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

Concentrated sulfuric acid (25 mL) and 2-amino-6-chloro-nicotinic acid (4.3 g, 25 mmol) described in Manufacturing Example 26-1-1 were added to methanol (50 mL) on an ice bath, and stirred at 70° C. for 5 hours. The reaction mixture was cooled and then neutralized by addition of aqueous sodium hydrogen carbonate (90 g) solution. The precipitated solids were filtered to obtain the title compound (3.2 g, 17 mmol, 68%).

後処理

  1. temperatureThe reaction mixture was cooled
  2. filtrationThe precipitated solids were filtered

出典と根拠

ORDレコード
ord-18895427fbde43ce970f88e3db762416
出典データセット
uspto-grants-2014_09
特許番号
US08841327B2

反応ノート

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