Methanol → Methyl 5-chloropyridine-3-carboxylate

HRID 877615

反応式

HRID 877615 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].S(=O)(=O)(O)O.[CH3:16]O>>[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([O:9][CH3:16])=[O:8]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 2479865-Chloronicotinic acid

生成物 1

HCID 15421663Methyl 5-chloropyridine-3-carboxylate

実験手順

5-Chloronicotinic acid (200 mg, 1.269 mmol) was refluxed overnight in the presence of concentrated sulfuric acid (8.20 mg, 0.063 mmol) in methanol (10 mL) at 70° C. The reaction was monitored by TLC. After completion of the reaction, the solvent was removed by vacuum and the compound was purified by column chromatography affording the title compound (120 mg). 1H NMR (400 MHz, CDCl3): δ 9.07 (d, 1H, J=1.6 Hz), 8.72 (d, 1H, J=2.0 Hz), 8.26 (m, 1H), 3.95 (s, 1H).

後処理

  1. customAfter completion of the reaction
  2. customthe solvent was removed by vacuum
  3. customthe compound was purified by column chromatography

出典と根拠

ORDレコード
ord-42809225335142fc9e035820c45dcc12
出典データセット
uspto-grants-2015_03
特許番号
US08987335B2

関連ノート

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