Hydrochloric Acid → HCID 178461412, Verbindung

Temperatur

0 °C

To a mixture of Example 168C (0.10 g, 0.325 mmol) in 2 mL of water was added 1.5 mL 6 M HCl. The resulting solution was cooled to 0° C. and NaNO2 (0.034 g, 0.488 mmol), dissolved in 1 mL water, was added dropwise. The resulting mixture was stirred for 30 minutes at 0° C. and subsequently heated to 90° C. for one hour. After cooling, contents were filtered and the precipitate was washed with 10 mL water and dried under reduced pressure to provide the product in 47% yield as a brown solid in HCl salt form, which was used without further purification. 1H NMR (CD3OD, 300 MHz) δ 8.10 (d, J=9 Hz, 1H), 7.82 (d, J=3 Hz, 1H), 7.60 (dd, J=3, 9 Hz, 1H), 3.89–3.76 (m, 2H), 3.58–3.53 (m, 1H) 3.42–3.23 (m, 4H), 2.38–2.30 (m, 1H), 2.16–2.06 (m, 2H), 1.83–1.75 (m, 1H), 1.51 (d, J=6 Hz, 3H). MS (ESI) [M]+ at 336.

1. additionwas added dropwise
2. temperaturesubsequently heated to 90° C. for one hour
3. temperatureAfter cooling
4. filtrationcontents were filtered
5. washthe precipitate was washed with 10 mL water
6. customdried under reduced pressure
7. customto provide the product in 47% yield as a brown solid in HCl salt form, which
8. customwas used without further purification

ORD-Eintrag

ord-5210a7a94a3945ae86f271c04fc36674

Quelldatensatz

uspto-grants-2006_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07153889B2