Hydrochloric Acid → HCID 178428133、化合物

HRID 1700761ノート

反応式

HRID 1700761 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH:9]1[CH2:18][C:17]2[N:16]=[CH:15][CH:14]=[C:13]([CH3:19])[C:12]=2[C:11](=O)[CH2:10]1.[C:21]([NH:24][NH2:25])([NH2:23])=[NH:22].Cl.Cl.O>C(O)C>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH:9]1[CH2:18][C:17]2[N:16]=[CH:15][CH:14]=[C:13]([CH3:19])[C:12]=2[C:11](=[N:25][NH:24][C:21]([NH2:23])=[NH:22])[CH2:10]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 117482737-(2-Chloro-5-fluorophenyl)-4-methyl-5,6,7,8-tetrahydroquinolin-5-oneHCID 178418668HCID 178418668、化合物

生成物 1

HCID 178428133HCID 178428133、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 7-(2-chloro-5-fluorophenyl)-4-methyl-5,6,7,8-tetrahydroquinolin-5-one in ethanol (10 ml) were added aminoguanidine hydrochloride (0.041 g), concentrated hydrochloric acid (0.078 ml) and water (0.078 ml), and the mixture was refluxed for 4 hours. Under reduced pressure, the solvent was evaporated, and to the residue was added water. The aqueous layer was washed with ethyl acetate, and to the aqueous layer was added sodium hydrogen carbonate solution to make it alkaline. The solution was extracted with ethyl acetate, and the organic layer was washed with water and saturated brine, dried with magnesium sulfate, and concentrated under reduced pressure. The residue was dissolved in 1N hydrochloric acid (1 ml) and concentrated to give crystals, which were recrystallized from ethanol-ethyl acetate to give 7-(2-chloro-5-fluorophenyl)-5-guanidinoimino-4-methyl-5,6,7,8-tetrahydroquinoline hydrochloride (Compound 170) (0.05 g) as colorless crystals.

後処理

  1. temperaturethe mixture was refluxed for 4 hours
  2. customUnder reduced pressure, the solvent was evaporated
  3. additionto the residue was added water
  4. washThe aqueous layer was washed with ethyl acetate
  5. additionto the aqueous layer was added sodium hydrogen carbonate solution
  6. extractionThe solution was extracted with ethyl acetate
  7. washthe organic layer was washed with water and saturated brine
  8. dry with materialdried with magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. dissolutionThe residue was dissolved in 1N hydrochloric acid (1 ml)
  11. concentrationconcentrated
  12. customto give crystals, which
  13. customwere recrystallized from ethanol-ethyl acetate

出典と根拠

ORDレコード
ord-5057302196a64907b85fa347a63f6648
出典データセット
uspto-grants-2002_02
特許番号
US06350749B1

反応ノート

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