Hydrochloric Acid → HCID 178430222、化合物

HRID 1700532ノート

反応式

HRID 1700532 の反応式
[CH3:1][N:2]1[C:10]2[CH2:9][CH:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH2:7][C:6](=O)[C:5]=2[C:4]([CH3:18])=[CH:3]1.[C:19]([NH:22][NH2:23])([NH2:21])=[NH:20].[ClH:24].Cl.O>C(O)C>[ClH:24].[NH:22]([N:23]=[C:6]1[CH2:7][CH:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:9][C:10]2[N:2]([CH3:1])[CH:3]=[C:4]([CH3:18])[C:5]1=2)[C:19]([NH2:21])=[NH:20]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 18317454HCID 18317454、化合物HCID 178418668HCID 178418668、化合物

生成物 1

HCID 178430222HCID 178430222、化合物収率 23.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1,3-dimethyl-6-phenyl-4,5,6,7-tetrahydroindol-4-one (0.31 g), aminoguanidine hydrochloride (0.15 g), concentrated hydrochloric acid (0.065 ml), water (0.065 ml) and ethanol (50 ml) was refluxed for 5 hours. Under reduced pressure, the solvent was evaporated, and the residue was dissolved in water. The solution was washed with diethylether, and to the mixture was added sodium hydrogen carbonate solution. The mixture was extracted with ethyl acetate, and the organic layer was dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was dissolved in ethanol. To the solution was added 1N hydrochloric acid. The solvent was evaporated, and the residue was recrystallized from ethanol-ethyl acetate to give 4-guanidinoimino-1,3-dimethyl-6-phenyl-4,5,6,7-tetrahydroindole hydrochloride (Compound 8) (0.1 g) as colorless crystals.

後処理

  1. temperaturewas refluxed for 5 hours
  2. customUnder reduced pressure, the solvent was evaporated
  3. dissolutionthe residue was dissolved in water
  4. washThe solution was washed with diethylether
  5. additionto the mixture was added sodium hydrogen carbonate solution
  6. extractionThe mixture was extracted with ethyl acetate
  7. dry with materialthe organic layer was dried with magnesium sulfate
  8. customUnder reduced pressure, the solvent was evaporated
  9. dissolutionthe residue was dissolved in ethanol
  10. additionTo the solution was added 1N hydrochloric acid
  11. customThe solvent was evaporated
  12. customthe residue was recrystallized from ethanol-ethyl acetate

出典と根拠

ORDレコード
ord-9f9f0562436b4bea9b39fd7a202f1f05
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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