Methanol → Methyl 2-chloro-6-methoxyisonicotinate

HRID 245078ノート

反応式

HRID 245078 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([O:11][CH3:12])[N:10]=1)[C:5]([OH:7])=[O:6].[CH3:13]O>OS(O)(=O)=O>[CH3:13][O:6][C:5](=[O:7])[C:4]1[CH:8]=[C:9]([O:11][CH3:12])[N:10]=[C:2]([Cl:1])[CH:3]=1

参加物

4

反応物 2

HCID 887MethanolHCID 27821242-Chloro-6-methoxypyridine-4-carboxylic acid

生成物 1

HCID 13339618Methyl 2-chloro-6-methoxyisonicotinate

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
0 °C

実験手順

To a suspension of 2-chloro-6-methoxy-isonicotinic acid (244 g, 1.30 mol) in methanol (2.5 L), H2SO4 (20 mL) is added. The mixture is stirred at reflux for 24 h before it is cooled to 0° C. The solid material is collected, washed with methanol (200 mL) and water (500 mL) and dried under HV to give 2-chloro-6-methoxy-isonicotinic acid methyl ester (165 g) as a white solid; LC-MS: tR=0.94 min, [M+1]+=201.89.

後処理

  1. additionis added
  2. temperatureat reflux for 24 h before it
  3. customThe solid material is collected
  4. washwashed with methanol (200 mL) and water (500 mL)
  5. customdried under HV

出典と根拠

ORDレコード
ord-0a7cf0719f6146c0aaeb39853efd8457
出典データセット
uspto-grants-2014_02
特許番号
US08658675B2

反応ノート

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