Methanol → Methyl 2-chloro-6-methoxyisonicotinate

HRID 732407

反応式

HRID 732407 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].S(=O)(=O)(O)O.[CH3:18]O>>[CH3:18][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 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 27821242-Chloro-6-methoxypyridine-4-carboxylic acid

生成物 1

HCID 13339618Methyl 2-chloro-6-methoxyisonicotinate

実験手順

Mix commercially available 2-chloro-6-methoxy-isonicotinic acid (17 g, 90.6 mmol), concentrated sulfuric acid (0.85 mL) in methanol (150 mL) and reflux overnight. Cool the mixture to room temperature, filter and dry the solid under vacuum to give the title compound (15.5 g). Concentrate filtrate and dilute with ethyl acetate (150 mL). Wash with sodium bicarbonate solution, water, dry (sodium sulfate) and concentrate to give additional title compound (1.7 g) (17.2 g, 93% combined yield).

後処理

  1. temperaturereflux overnight
  2. filtrationfilter
  3. customdry the solid under vacuum

出典と根拠

ORDレコード
ord-54369f18103945da97ca1f5f8227fed3
出典データセット
uspto-grants-2009_09
特許番号
US07585885B2

関連ノート

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