Dimethylformamide → HCID 58255175, compound

Under nitrogen, to a solution of 2-bromobutanoic acid (2.0 g, 12.0 mmol) in DCM (50 mL) at 0° C. were sequentially added thionyl chloride (2.6 mL, 35.9 mmol) and 0.5 mL of DMF. The reaction was allowed to warm to room temperature and was stirred overnight. The reaction mixture was concentrated in vacuo and then cooled to 0° C. Thirty (30) mL of 40% ethylamine water solution was added slowly. The reaction was allowed to warm to room temperature and was stirred for 2 h, followed by extraction with EtOAc. The combined organic extracts were dried (Na2SO4), and concentrated in vacuo to afford 2-bromo-N-ethylbutanamide.

1. customat 0° C.
2. concentrationThe reaction mixture was concentrated in vacuo
3. temperaturecooled to 0° C
4. additionThirty (30) mL of 40% ethylamine water solution was added slowly
5. temperatureto warm to room temperature
6. stirringwas stirred for 2 h
7. extractionfollowed by extraction with EtOAc
8. dry with materialThe combined organic extracts were dried (Na2SO4)
9. concentrationconcentrated in vacuo

ORD record

ord-ba01ea24addb47acb8aabf7a2ca2a62c

Source dataset

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08859574B2