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Hydrochloric Acid → N-Methyl-1-[5-phenyl-1-(2-thienylsulfonyl)-1H-pyrrol-3-yl]methanamine hydrochloride

HRID 554412
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 554412
[C:1]1([C:7]2[N:11]([S:12]([C:15]3[S:16][CH:17]=[CH:18][CH:19]=3)(=[O:14])=[O:13])[CH:10]=[C:9]([CH:20]=O)[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.[CH3:24][NH2:25].[BH4-].[Na+].[ClH:28].C(=O)([O-])O.[Na+]>CO>[ClH:28].[CH3:24][NH:25][CH2:20][C:9]1[CH:8]=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[N:11]([S:12]([C:15]2[S:16][CH:17]=[CH:18][CH:19]=2)(=[O:14])=[O:13])[CH:10]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 57454252Monomethylamine methanolHCID 862328445-Phenyl-1-(2-thienylsulfonyl)-1H-pyrrole-3-carbaldehyde

Produkt 1

HCID 57522260
N-Methyl-1-[5-phenyl-1-(2-thienylsulfonyl)-1H-pyrrol-3-yl]methanamine hydrochloride
Ausbeute 82 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

5-Phenyl-1-(2-thienylsulfonyl)-1H-pyrrole-3-carbaldehyde (180 mg) was dissolved in methanol (20 mL), a 40% methylamine methanol solution (220 mg) was added at room temperature, and the mixture was stirred for 30 min. Sodium borohydride (64 mg) was added at room temperature, and the mixture was stirred for 10 min. 1 mol/L Hydrochloric acid (20 mL) was added, and the mixture was stirred for 5 min. The reaction mixture was alkalized with a saturated aqueous sodium hydrogencarbonate solution and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (eluent: hexane-ethyl acetate=1:4→0:1), and dissolved in ethyl acetate (5 mL). A 4 mol/L hydrogen chloride-ethyl acetate solution (1 mL) was added, and the mixture was concentrated under reduced pressure. The residue was crystallized from ethyl acetate to give the title compound as colorless crystals (yield 171 mg, 82%).

Aufarbeitung

  1. stirringthe mixture was stirred for 10 min
  2. stirringthe mixture was stirred for 5 min
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by basic silica gel column chromatography (eluent: hexane-ethyl acetate=1:4→0:1)
  8. dissolutiondissolved in ethyl acetate (5 mL)
  9. additionA 4 mol/L hydrogen chloride-ethyl acetate solution (1 mL) was added
  10. concentrationthe mixture was concentrated under reduced pressure
  11. customThe residue was crystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-4795bb3b3ef548dfb1431bba67631bbc
Quelldatensatz
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08048909B2

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