Acetic Acid → 3-(Dimethylaminomethyl)-2-(methoxycarbonylamino)-6-(phenylthio) imidazo [1,2-a] pyridine

HRID 1413431ノート

反応式

HRID 1413431 の反応式
[CH3:1][O:2][C:3]([NH:5][C:6]1[N:7]=[C:8]2[CH:13]=[CH:12][C:11]([S:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[CH:10][N:9]2[CH:21]=1)=[O:4].[CH3:22][NH:23][CH3:24].C=O.[C:27](O)(=O)C>C(=O)(O)[O-].[Na+]>[CH3:22][N:23]([CH2:27][C:21]1[N:9]2[CH:10]=[C:11]([S:14][C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:12]=[CH:13][C:8]2=[N:7][C:6]=1[NH:5][C:3]([O:2][CH3:1])=[O:4])[CH3:24]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 674DimethylamineHCID 712FormaldehydeHCID 12414300Methyl [6-(phenylsulfanyl)imidazo[1,2-a]pyridin-2-yl]carbamate

生成物 1

HCID 545555143-(Dimethylaminomethyl)-2-(methoxycarbonylamino)-6-(phenylthio) imidazo [1,2-a] pyridine

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒

実験手順

2-(Methoxycarbonylamino)-6-(phenylthio) imidazo [1,2-a] pyridine (0.75 gm.) is added to a solution of 50% aqueous dimethylamine (0.215 gm., 37% formaldehyde (0.19 gm.) and acetic acid (0.35 g.) and heated at 50° C. for 3 hours. After cooling, the reaction mixture is diluted with aqueous sodium bicarbonate and the resultant precipitate is collected by filtration. After drying, the crude product is recrystallized from ethyl acetate to yield 3-(dimethylaminomethyl)-2-(methoxycarbonylamino)-6-(phenylthio) imidazo [1,2-a] pyridine m.p. 172°-175° C.

後処理

  1. temperatureAfter cooling
  2. filtrationthe resultant precipitate is collected by filtration
  3. customAfter drying
  4. customthe crude product is recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-05dabc1b73884d4f8fca533e33e4d804
出典データセット
uspto-grants-1981_02
特許番号
US04250174

反応ノート

読み込み中…