Perchloric Acid → O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine

HRID 44117

Reaktionsgleichung

Reaktionsgleichung von HRID 44117
[C:1]1([CH3:19])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[S:9]([O:12][N:13]=C(OCC)C)(=[O:11])=[O:10].Cl(O)(=O)(=O)=O>O1CCOCC1>[C:1]1([CH3:19])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[S:9]([O:12][NH2:13])(=[O:11])=[O:10]

Komponenten

4

Edukt 2

HCID 24247Perchloric AcidHCID 2724212Ethyl N-[[(2,4,6-trimethylphenyl)sulfonyl]oxy]ethanimidate

Produkt 1

HCID 11830845O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Ethyl N-mesitylsulfonyloxyacetimidate (20 g, 65.7 mmol, 1 eq) was dissolved in 1,4-dioxane (6 ml) and the solution was cooled to 0° C. To the mixture was added dropwise Perchloric acid (10 m), and the reaction mixture was then stirred at 0° C. for 45 minutes. The solution was poured into ice water, and the solid precipitated was filtered and washed with water and dried for 15 minutes in vacuum. The sample was stored in plastic container at −20° C. 1HNMR (400 MHz, DMSO-d6): δ 2.32 (s, 3H), 2.64 (s, 6H), 4.98 (br peak, 2H), 6.99 (s, 2H).

Aufarbeitung

  1. customthe solid precipitated
  2. filtrationwas filtered
  3. washwashed with water
  4. customdried for 15 minutes in vacuum
  5. customwas stored in plastic container at −20° C

Quellen und Nachweise

ORD-Eintrag
ord-31874d42e9e246259412665d9e168059
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08536338B2

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