Methanol → Triethylamine, 2',2''-dichloro-1,1-dimethyl-

Temperatur

20 °C

Thionyl chloride (30 mL, 409.2 mmol) was diluted in chloroform (40 mL) and stirred at 20° C. 2,2′-(Tert-butylazanediyl)diethanol (30 g, 186 mmol) in chloroform (20 mL) was added dropwise over 45 minutes. The resulting mixture was stirred for 18 hours at 20° C. and refluxed for 2 hours. The mixture was cooled and methanol (˜10 mL) was added, followed by ethyl ether (˜50 mL). The resulting precipitate was filtered, washed with ethyl ether and dried under vacuum to give the title material (35 g, 81%) as the HCl salt. 1H NMR (400 MHz, CDCl3) δ ppm: 1.60 (9H, s), 3.20 (2H, s), 3.68 (2H, s), 4.12-4.19 (2H, m), 4.21-4.28 (2H, m), 12.66 (1H, s).

1. stirringThe resulting mixture was stirred for 18 hours at 20° C.
2. temperaturerefluxed for 2 hours
3. temperatureThe mixture was cooled
4. filtrationThe resulting precipitate was filtered
5. washwashed with ethyl ether
6. customdried under vacuum

ORD-Eintrag

ord-1ed2bc57db354d7186cb826431b64268

Quelldatensatz

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08343999B2