4-Hydroxybenzaldehyde → HCID 22344627、化合物

HRID 2299725ノート

反応式

HRID 2299725 の反応式
Cl.[Cl:2][C:3]1[N:8]2[CH:9]=[C:10]([CH2:12]Cl)[N:11]=[C:7]2[CH:6]=[CH:5][CH:4]=1.[OH:14][C:15]1[CH:22]=[CH:21][C:18]([CH:19]=[O:20])=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[Cl:2][C:3]1[N:8]2[CH:9]=[C:10]([CH2:12][O:14][C:15]3[CH:22]=[CH:21][C:18]([CH:19]=[O:20])=[CH:17][CH:16]=3)[N:11]=[C:7]2[CH:6]=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 1264-HydroxybenzaldehydeHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 223446015-Chloro-2-(chloromethyl)imidazo(1,2-a)pyridine hydrochloride

生成物 1

HCID 22344627HCID 22344627、化合物収率 98%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 5-chloro-2-(chloromethyl)imidazo[1,2-a]pyridine hydrochloride (3.00 g), 4-hydroxybenzaldehyde (1.81 g), potassium carbonate (6.14 g) and N,N-dimethylformamide (30 ml) was stirred at room temperature for 15 hours, poured into water and extracted with ethyl acetate. The ethyl acetate layer was washed with an queous saturated solution of sodium chloride, dried (MgSO4) and concentrated. The remaining crystals were recrystallized from ethyl acetate-hexane to obtain 4-(5-chloroimidazo[1,2-a]pyridin-2-ylmethoxy)benzaldehyde (3.55 g, yield 98%) as colorless crystals. m.p. 126-130° C.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with an queous saturated solution of sodium chloride
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customThe remaining crystals were recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-48edce69a6ae49c4b7953dc3a86d7f52
出典データセット
uspto-grants-2002_12
特許番号
US06495581B1

反応ノート

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