Hydrochloric Acid → HCID 21873953、化合物

HRID 723397ノート

反応式

HRID 723397 の反応式
[NH2:1][C:2]1[C:3]2[N:4]([C:17]([CH3:21])=[C:18]([CH3:20])[N:19]=2)[CH:5]=[CH:6][C:7]=1[C:8](=[O:16])[CH:9]=[CH:10][C:11]1[CH:15]=[CH:14][S:13][CH:12]=1.[OH-:22].[Na+].OO.Cl>C(O)C>[NH2:1][C:2]1[C:3]2[N:4]([C:17]([CH3:21])=[C:18]([CH3:20])[N:19]=2)[CH:5]=[CH:6][C:7]=1[C:8](=[O:16])[CH:9]1[O:22][CH:10]1[C:11]1[CH:15]=[CH:14][S:13][CH:12]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 69586325HCID 69586325、化合物

生成物 1

HCID 21873953HCID 21873953、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A suspension of 2.6 9 of 8-amino-2,3-dimethyl-7-[3-(3-thienyl)-1-oxo-2-propenyl]imidazo[1,2-a]pyridine in 80 ml of ethanol is treated successively with 5.2 ml of 6 N aqueous sodium hydroxide solution and 5 ml of 30% strength aqueous hydrogen peroxide solution, stirred at room temperature for 48 hours, poured onto 200 ml of ice water and adjusted to pH 7–8 with semisatd. aqueous hydrochloric acid. The mixture is then extracted three times with 100 ml of dichloromethane each time, the combined organic phases are washed once with saturated sodium thiosulfate solution and once with 100 ml of distilled water, the solvent is stripped off in vacuo and the residue is purified on silica gel (eluent:methylene chloride/methanol=100/3). 1.2 g of the title compound of m.p. 186–89° C. (diethyl ether) are obtained.

後処理

  1. extractionThe mixture is then extracted three times with 100 ml of dichloromethane each time
  2. washthe combined organic phases are washed once with saturated sodium thiosulfate solution and once with 100 ml of distilled water
  3. customthe residue is purified on silica gel (eluent:methylene chloride/methanol=100/3)

出典と根拠

ORDレコード
ord-171c934231f940f6b9ed749f6e6c25ad
出典データセット
uspto-grants-2006_11
特許番号
US07141567B2

反応ノート

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