Hydrochloric Acid → 8-[(3,5-Difluoropyridine-4-yl)methoxy]-2,6-dimethylimidazo[1,2-a]pyridine-3-carboxylic acid

HRID 1844193ノート

反応式

HRID 1844193 の反応式
[F:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([F:26])[C:7]=1[CH2:8][O:9][C:10]1[C:11]2[N:12]([C:17]([C:21]([O:23]CC)=[O:22])=[C:18]([CH3:20])[N:19]=2)[CH:13]=[C:14]([CH3:16])[CH:15]=1.[OH-].[Na+].Cl>O1CCOCC1>[F:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([F:26])[C:7]=1[CH2:8][O:9][C:10]1[C:11]2[N:12]([C:17]([C:21]([OH:23])=[O:22])=[C:18]([CH3:20])[N:19]=2)[CH:13]=[C:14]([CH3:16])[CH:15]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86718219Ethyl 8-[(3,5-difluoropyridine-4-yl)methoxy]-2,6-dimethylimidazo[1,2-a]pyridine-3-carboxylate

生成物 1

HCID 867182208-[(3,5-Difluoropyridine-4-yl)methoxy]-2,6-dimethylimidazo[1,2-a]pyridine-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

5.34 g (14.78 mmol) of ethyl 8-[(3,5-difluoropyridine-4-yl)methoxy]-2,6-dimethylimidazo[1,2-a]pyridine-3-carboxylate from Example 130A were initially charged in 160 ml of dioxane, 147.8 ml (147.8 mmol) of 1 M aqueous sodium hydroxide solution were added and the mixture was stirred at RT overnight. The reaction mixture, cooled to RT, was adjusted to about pH 4 using 1 N aqueous hydrochloric acid, the solvent was concentrated to half of its original volume and the precipitated solid was filtered off with suction and dried under reduced pressure. This gave 4.61 g (93% of theory) of the target compound.

後処理

  1. temperatureThe reaction mixture, cooled to RT
  2. concentrationthe solvent was concentrated to half of its original volume
  3. filtrationthe precipitated solid was filtered off with suction
  4. customdried under reduced pressure

出典と根拠

ORDレコード
ord-ef5eb163bf454661966ba90f38cd757e
出典データセット
uspto-grants-2015_02
特許番号
US08946215B2

反応ノート

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