Malonic Acid → (2E)-3-(4-Bromo-2-thienyl)-2-propenoic acid

Temperatur

100 °C

4-Bromothiophenecarboxaldehyde (2.5 g, 13.1 mmol) was placed in a 25 ml round bottomed flask and charged with piperidine (0.14 ml, 0.11 mmol) and pyridine (7.1 ml). Malonic acid was then added (2.21 mg, 21.2 mmol) and the reaction heated to 100° C. and maintained for 24 h. The reaction was then allowed to cool to room temperature and the solvent removed in vacuo. The remaining residue was acidified with concentrated HCl to pH 3 and the solid collected, filtered and washed with distilled water (20 ml). It was then air and oven dried to yield a yellow solid (3.04 g, 100%).

1. temperaturemaintained for 24 h
2. temperatureto cool to room temperature
3. customthe solvent removed in vacuo
4. customthe solid collected
5. filtrationfiltered
6. washwashed with distilled water (20 ml)
7. customair and oven dried

ORD-Eintrag

ord-e00c48da84954c9fa3482e6fb06556eb

Quelldatensatz

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09216992B2