Pyridine → HCID 641127, compound

To a solution of 2,2,2-trichloroacetyl chloride (10.6 g, 6.52 mL, 58.1 mmol) in dichloromethane (15 mL) cooled to −10° C. was added a mixture of (E)-1-ethoxyprop-1-ene (5 g, 6.43 mL, 58.1 mmol) and pyridine (4.59 g, 4.7 mL, 58.1 mmol) over a period of 15 min. After the addition was complete, the mixture was stirred at RT for 16 h. The resulting precipitate was filtered and washed with dichloromethane. The filtrate was concentrated in vacuo and dried at 40° C. in high vacuum to give the product as brown semisolid (16.1 g with 80% purity, 95.8%). The crude material was used directly in the next step without any further purification.

1. additionwas added
2. additionAfter the addition
3. filtrationThe resulting precipitate was filtered
4. washwashed with dichloromethane
5. concentrationThe filtrate was concentrated in vacuo
6. customdried at 40° C. in high vacuum

ORD record

ord-a21542612aa94922858a0276499f6f76

Source dataset

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08772510B2