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

HRID 1844193노트

반응식

HRID 1844193 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ef5eb163bf454661966ba90f38cd757e
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946215B2

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