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Hydrochloric Acid → HCID 22033496, Verbindung

HRID 325026
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 325026
O.[NH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH2:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]#[N:19])=[CH:14][CH:13]=2)[CH:4]=1.Cl.[C:21]1([S:27](Cl)(=[O:29])=[O:28])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>N1C=CC=CC=1>[C:18]([C:15]1[CH:14]=[CH:13][C:12]([CH2:11][CH2:10][O:9][C:5]2[CH:4]=[C:3]([NH:2][S:27]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)(=[O:29])=[O:28])[CH:8]=[CH:7][CH:6]=2)=[CH:17][CH:16]=1)#[N:19]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 7369Benzenesulfonyl chlorideHCID 22033543HCID 22033543, Verbindung

Produkt 1

HCID 22033496HCID 22033496, VerbindungAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049
Pyridine
Lösungsmittel

Versuchsvorschrift

To a cold (ice:water temperature) solution of amino-3-[2-(4-cyanophenyl)ethoxy]benzene×HCl (231 mg; 0.84 mmol; from step (iii) above) in pyridine (2 mL) was added benzenesulfonyl chloride (119 μL; 0.93 mmol) and the mixture was allowed to reach room temperature and stirred for three days. The pyridine was removed by evaporation and the residue was partitioned between water and EtOAc. The phases was separated and the water phase was extracted twice with EtOAc and the combined organic phase was washed once with 1M KHSO4, brine and dried (Na2SO4). The solvent was evaporated and the residue was subjected to purification by flash chromatography using a stepwise gradient of toluene:EtOAc (100:0, 90:10, 80:20, 60:40 and 40:60) as eluent to give 277 mg (87%) of the sub-title compound.

Aufarbeitung

  1. customto reach room temperature
  2. customThe pyridine was removed by evaporation
  3. customthe residue was partitioned between water and EtOAc
  4. customThe phases was separated
  5. extractionthe water phase was extracted twice with EtOAc
  6. washthe combined organic phase was washed once with 1M KHSO4, brine
  7. dry with materialdried (Na2SO4)
  8. customThe solvent was evaporated
  9. customthe residue was subjected to purification by flash chromatography

Quellen und Nachweise

ORD-Eintrag
ord-271f1c96ccb64c6791bf5e8dd395f479
Quelldatensatz
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06221898B1

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