Hydrochloric Acid → HCID 21873953, 화합물

HRID 723397노트

반응식

HRID 723397 반응식
[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

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 69586325HCID 69586325, 화합물

생성물 1

HCID 21873953HCID 21873953, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-171c934231f940f6b9ed749f6e6c25ad
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07141567B2

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