Methanol → 6-Methoxynicotinic acid

HRID 235850

反応式

HRID 235850 の反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([C:8]([OH:10])=[O:9])=[CH:4][CH:3]=1.[CH3:11][OH:12]>C[O-].[Na+]>[CH3:11][O:12][C:2]1[N:7]=[CH:6][C:5]([C:8]([OH:10])=[O:9])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 887MethanolHCID 792226-Chloronicotinic acid

生成物 1

HCID 5924996-Methoxynicotinic acid

試薬・触媒・溶媒 1

HCID 10942334Sodium Methoxide溶媒

実験手順

To a suspension of 6-chloropyridine-3-carboxylic acid (4.15 g) in methanol (40 cc), 4 M methanolic sodium methylate solution (40 cc) is added. The mixture is heated under reflux for 60 hours. The solvent is distilled off under reduced pressure (4 kPa). The residue is taken up in distilled water (100 cc) and the mixture is acidified to pH 5 with hydrochloric acid in 11.9 M aqueous solution. The precipitate produced is separated by filtration, washed with distilled water (5×10 cc) and dried in the air. 6-Methoxypyridine-3-carboxylic acid (3.3 g) is produced, m.p. 180° C.

後処理

  1. additionis added
  2. temperatureThe mixture is heated
  3. temperatureunder reflux for 60 hours
  4. distillationThe solvent is distilled off under reduced pressure (4 kPa)
  5. customThe precipitate produced
  6. customis separated by filtration
  7. washwashed with distilled water (5×10 cc)
  8. customdried in the air

出典と根拠

ORDレコード
ord-25f2f5f4775e4709968269a240fc8baa
出典データセット
uspto-grants-1987_02
特許番号
US04642308

関連ノート

読み込み中…