Hydrochloric Acid → HCID 57448161, 화합물

To 1A (1.50 g, 7.25 mmol) in refluxing THF (72 mL) was added a 2M THF solution of BH3.SMe2 (10.8 mL, 21.7 mmol). After heating at reflux for 2 h, the reaction was cooled to rt and 6M HCl (4.32 mL) was slowly added. The reaction was heated to reflux for 30 min, then cooled to rt, concentrated and azeotroped (3×) with THF/MeOH on a rotary evaporator. The resulting residue was taken up in THF and filtered to provide 1B (1.40 g, 79%) as a white solid. 1H NMR (400 MHz, CD3OD) δ ppm 1.15 (m, 2H) 1.29 (m, 2H) 2.91 (m, 1H) 4.52 (s, 2H) 7.72 (m, J=7.69, 7.69 Hz, 2H) 7.80 (t, J=6.81 Hz, 1H) 8.04 (d, J=7.91 Hz, 1H).

1. temperatureAfter heating
2. temperatureat reflux for 2 h
3. temperatureThe reaction was heated
4. temperatureto reflux for 30 min
5. temperaturecooled to rt
6. concentrationconcentrated
7. customazeotroped (3×) with THF/MeOH
8. customon a rotary evaporator
9. filtrationfiltered

ORD 기록

ord-98c0fe9cac714b6d91868400869e3df4

출처 데이터셋

uspto-grants-2011_10

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08044242B2