Ammonia → HCID 89876230, Verbindung

HRID 594102

Reaktionsgleichung

Reaktionsgleichung von HRID 594102
[CH3:1][C:2]1[C:6]([CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([S:15](Cl)(=[O:17])=[O:16])=[CH:11][CH:10]=2)=[C:5]([CH3:19])[O:4][N:3]=1.[NH3:20]>CO>[CH3:1][C:2]1[C:6]([CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([S:15]([NH2:20])(=[O:17])=[O:16])=[CH:11][CH:10]=2)=[C:5]([CH3:19])[O:4][N:3]=1

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 164907024-((3,5-Dimethylisoxazol-4-yl)methoxy)benzene-1-sulfonyl chloride

Produkt 1

HCID 89876230HCID 89876230, VerbindungAusbeute 69,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

4-{[(3,5-dimethyl-4-isoxazolyl)methyl]oxy}benzenesulfonyl chloride (300 mg, 0.994 mmol) was added to ammonia solution (2 mL, 92 mmol, 0.88 NH3 in water). The reaction was stirred at 20° C. for 30 minutes, then left to stand overnight. The reaction mixture was diluted with methanol (5 mL) and passed sequentially through two separate aminopropyl (NH2) solid phase extraction (SPE) cartridges eluting with methanol. The product-containing fractions were combined and evaporated in vacuo to give product as a yellow solid (196.2 mg). LCMS (2 min, formic) Rt 0.71 min, m/z (ES+) 283 (M+H).

Aufarbeitung

  1. waitleft
  2. waitto stand overnight
  3. customseparate
  4. extractionaminopropyl (NH2) solid phase extraction (SPE) cartridges
  5. washeluting with methanol
  6. customevaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b44f110019724f3fb620e6ff3114cbd1
Quelldatensatz
uspto-grants-2016_01
Patentnummer
US09242972B2

Verknüpfte Notizen

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