Ethylamine → HCID 44469451, Verbindung

HRID 38896Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 38896
CC1C=CC(S(O[CH2:12][CH:13]2[O:18][C:17]3[CH:19]=[C:20]([S:23]([CH3:26])(=[O:25])=[O:24])[CH:21]=[CH:22][C:16]=3[O:15][CH2:14]2)(=O)=O)=CC=1.[CH2:27]([NH2:29])[CH3:28]>C(#N)C>[CH3:26][S:23]([C:20]1[CH:21]=[CH:22][C:16]2[O:15][CH2:14][CH:13]([CH2:12][NH:29][CH2:27][CH3:28])[O:18][C:17]=2[CH:19]=1)(=[O:24])=[O:25]

Komponenten

4

Edukt 2

HCID 6341EthylamineHCID 86652933[7-(Methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate

Produkt 1

HCID 44469451HCID 44469451, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of [7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate (0.7 g, 1.8 mmol), ethanamine (1 ml, 70% in water) and ACN (3 ml) was heated under microwave radiation at 120° C. for 30 min. Purification on flash column chromatography and on SCX-3 column (TEA/MeOH). Yield: 0.4 g, 72%. The amine was converted to the hydrochloric acid salt and was crystallized from MeOH/Et2O. M.p. 261° C. MS m/z (rel. intensity, 70 eV) 271 (M+, 19), 226 (4), 207 (9), 79 (6), 58 (bp).

Aufarbeitung

  1. customPurification on flash column chromatography
  2. customwas crystallized from MeOH/Et2O

Quellen und Nachweise

ORD-Eintrag
ord-27bdb7f13fc74e059e3b537b3d00a4af
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524766B2

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