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Hydrochloric Acid → 4-{[1-(5-Chloro-3-methyl-1-benzofuran-2-yl)-3-methylbutyl]amino}benzoic acid

HRID 2091164
ノート
印刷プレビュー

反応式

HRID 2091164 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([CH:10](Cl)[CH2:11][CH:12]([CH3:14])[CH3:13])=[C:7]([CH3:16])[C:6]=2[CH:17]=1.[NH2:18][C:19]1[CH:28]=[CH:27][C:22]([C:23]([O:25]C)=[O:24])=[CH:21][CH:20]=1.[I-].[Na+].C(=O)([O-])[O-].[Na+].[Na+].Cl.[OH-].[Na+]>C(O)C.O1CCCC1.CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8]([CH:10]([NH:18][C:19]3[CH:28]=[CH:27][C:22]([C:23]([OH:25])=[O:24])=[CH:21][CH:20]=3)[CH2:11][CH:12]([CH3:14])[CH3:13])=[C:7]([CH3:16])[C:6]=2[CH:17]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 6

HCID 313Hydrochloric AcidHCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 12082Methyl 4-aminobenzoateHCID 14798Sodium HydroxideHCID 667784465-Chloro-2-(1-chloro-3-methylbutyl)-3-methyl-1-benzofuran

生成物 1

HCID 66777168
4-{[1-(5-Chloro-3-methyl-1-benzofuran-2-yl)-3-methylbutyl]amino}benzoic acid
収率 43%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

To a mixture of 5-chloro-2-(1-chloro-3-methylbutyl)-3-methyl-1-benzofuran (668 mg) synthesized above, methyl 4-aminobenzoate (410 mg), sodium iodide (737 mg) and N,N-dimethylformamide (10 mL) was added sodium carbonate (521 mg) and the mixture was stirred at 80° C. for 8 hr. 1N Hydrochloric acid was added to quench the reaction, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (15% ethyl acetate/hexane) to give a yellow oil. To a mixture of the obtained oil, tetrahydrofuran (10 mL) and ethanol (10 mL) was added 1N aqueous sodium hydroxide solution (10.0 mL), and the mixture was stirred with heating under reflux for 8 hr, and concentrated under reduced pressure. The residue was dissolved in water (20 mL), and 1N hydrochloric acid (10.0 mL) was added at 0° C. The resulting precipitate was collected by filtration to give the title object compound (394 mg, 43%) as a pale-yellow solid.

後処理

  1. customto quench
  2. customthe reaction
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (15% ethyl acetate/hexane)
  8. customto give a yellow oil
  9. stirringthe mixture was stirred
  10. temperaturewith heating
  11. temperatureunder reflux for 8 hr
  12. concentrationconcentrated under reduced pressure
  13. dissolutionThe residue was dissolved in water (20 mL)
  14. addition1N hydrochloric acid (10.0 mL) was added at 0° C
  15. filtrationThe resulting precipitate was collected by filtration

出典と根拠

ORDレコード
ord-f433c0ac6882438fa126f05a1f51f76e
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436043B2

反応ノート

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