Sulfuric Acid → HCID 21873976、化合物

HRID 985080ノート

反応式

HRID 985080 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.S(=O)(=O)(O)O.[OH-].[Na+]>>[CH3:20][C:18]1[N:19]=[C:3]2[C:2]3[NH:1][CH:10]([C:11]4[CH:15]=[CH:14][S:13][CH:12]=4)[CH2:9][C:8](=[O:16])[C:7]=3[CH:6]=[CH:5][N:4]2[C:17]=1[CH3:21]

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 69586325HCID 69586325、化合物

生成物 1

HCID 21873976HCID 21873976、化合物収率 69.2%

実験手順

2.6 g of 8-amino-2,3-dimethyl-7-[3-(3-thienyl)-1-oxo-2-propenyl]imidazo[1,2-a]pyridine are treated at room temperature with 20 ml of aqueous 70% strength sulfuric acid, poured onto ice water (100 ml) after 90 minutes, neutralized with aqueous 6 N sodium hydroxide solution and extracted three times with 50 ml of methylene chloride each time. The combined organic phases are washed with water, dried over sodium sulfate, the solvent is stripped off in vacuo and the remaining yellow oil is stirred with 15 ml of diethyl ether. The yellowish solid obtained here is filtered off and dried in vacuo. 1.8 g of the title compound of m.p. 176-77° C. (diethyl ether) are obtained.

後処理

  1. additionpoured onto ice water (100 ml) after 90 minutes
  2. extractionextracted three times with 50 ml of methylene chloride each time
  3. washThe combined organic phases are washed with water
  4. dry with materialdried over sodium sulfate
  5. customThe yellowish solid obtained here
  6. filtrationis filtered off
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-e566304a11bd4b63bc1faf0c835d369d
出典データセット
uspto-grants-2005_03
特許番号
US06869949B2

反応ノート

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