Ethanol → HCID 178434443, Verbindung

Temperatur

80 °C

Sodium acetate (166 mg, 2.02 mmol), thiosemicarbazide (333 mg, 3.66 mmol), 100 ml ethanol and 2 ml distilled water were charged into a 250 ml round bottom flask. The resulting suspension was heated to 80° C. until it becomes a clear solution. The reaction was then cooled down to room temperature and the resulting mixture was added into a 250 ml round bottom flask containing 3-methyl-1H-pyrazolo[3,4-b]pyridine-5-carbaldehyde (333 mg, 2.1 mmol). After the addition, the resulting mixture was heated to 80° C. for 16 hours. The mixture was cooled to room temperature and solid was precipitated out. The solid was filtered off and washed with ether (50 ml). The product (500 mg, y=95%) was used directly for the next step without further purification.

1. additionwere charged into a 250 ml round bottom flask
2. temperatureThe reaction was then cooled down to room temperature
3. additionthe resulting mixture was added into a 250 ml round bottom flask
4. additionAfter the addition
5. temperaturethe resulting mixture was heated to 80° C. for 16 hours
6. temperatureThe mixture was cooled to room temperature
7. customsolid was precipitated out
8. filtrationThe solid was filtered off
9. washwashed with ether (50 ml)
10. customThe product (500 mg, y=95%) was used directly for the next step without further purification

ORD-Eintrag

ord-40a5562e72914469a3ae5f1058fb23ad

Quelldatensatz

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07919514B2