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Hydroxyamine hydrochloride → N-Hydroxy-3-{3-[(naphthalen-1-ylmethyl)sulfamoyl]-phenyl)-acrylamide

HRID 226140
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 226140
Cl.[NH2:2][OH:3].C([O-])(O)=O.[Na+].[C:9]1([CH2:19][NH:20][S:21]([C:24]2[CH:25]=[C:26]([CH:30]=[CH:31][C:32](Cl)=[O:33])[CH:27]=[CH:28][CH:29]=2)(=[O:23])=[O:22])[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][CH:10]=1>O1CCCC1>[OH:3][NH:2][C:32](=[O:33])[CH:31]=[CH:30][C:26]1[CH:27]=[CH:28][CH:29]=[C:24]([S:21](=[O:23])(=[O:22])[NH:20][CH2:19][C:9]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH:12]=[CH:11][CH:10]=2)[CH:25]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 739894053-{3-[(Naphthalen-1-ylmethyl)-sulfamoyl]-phenyl}-acryloyl chloride

Produkt 1

HCID 85331087N-Hydroxy-3-{3-[(naphthalen-1-ylmethyl)sulfamoyl]-phenyl)-acrylamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a suspension of hydroxylamine-hydrochloride (0.30 g, 4.35 mmol) in tetrahydrofuran (6 ml) a saturated NaHCO3 solution (4 ml) was added and the resultant mixture was stirred at ambient temperature for 10 min. To the reaction mixture a solution of crude 3-{3-[(naphthalen-1-ylmethyl)-sulfamoyl]-phenyl}-acryloyl chloride (16a) (0.33 g) in tetrahydrofuran (4 ml) was added and the mixture was stirred at ambient temperature for one hour. The reaction mixture was partitioned between ethyl acetate and 2N HCl. The organic layer was washed successively with water and saturated NaCl, then the solvent was removed. The residue was crystallised from ethyl acetate-acetonitrile affording the title compound (0.13 g, 40%) as a lightly pink crystals. M.p. 177° C. 1H NMR (DMSO-d6, HMDSO) δ: 4.45 (2H, d, J=6.0 Hz); 6.58 (1H, d, J=16.0 Hz); 7.29-8.38 (13H, m); 9.12 (1H, br s); 10.83 (1H, br s). HPLC analysis on Symmetry C8 column: impurities 1.5% (column size 3.9×150 mm; mobile phase acetonitrile—0.1M phosphate buffer (pH 2.5), 40:60; sample concentration 0.25 mg/ml; flow rate 1.2 ml/min; detector UV 220 nm). Anal. Calcd for C20H18N2O4S, %: C 62.54, H 4.70, N, 7.21. Found, %: C 62.81, H 4.74, N 7.32.

Aufarbeitung

  1. additionwas added
  2. customThe reaction mixture was partitioned between ethyl acetate and 2N HCl
  3. washThe organic layer was washed successively with water and saturated NaCl
  4. customthe solvent was removed
  5. customThe residue was crystallised from ethyl acetate-acetonitrile affording the title compound (0.13 g, 40%) as a lightly pink crystals

Quellen und Nachweise

ORD-Eintrag
ord-40040597452549e49b3b6cd8ba67789b
Quelldatensatz
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07557140B2

Notizen zur Reaktion

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