Sulfuric Acid → HCID 66998207, compound

Temperature

0 °C

500 ml of THF were cooled to −72° C. and admixed at this temperature first with 31.9 g of diisopropylamine and then at the same temperature with 126 ml of n-BuLi (2.5 molar in hexane). Subsequently, 35.1 g of benzyl cyanide dissolved in a further 250 ml of THE were added dropwise within 1 h. The mixture was left to stir for a further 2 h in order to complete the formation of the anion. Subsequently, at −72° C., within 2 h, the mixture was admixed with a solution of 50 g of 1,1,1-trifluorobut-3-en-2-one and then left to stir at this temperature for 1 h. Subsequently, the mixture was warmed to 0° C. and, for neutralization, admixed with a solution of 16.1 g of sulphuric acid (96%) in 50 ml of water. Subsequently, 500 ml of toluene were added, the phases were separated and the aqueous phase was re-extracted twice with a further 100 ml of toluene. The combined organic phases were dried over sodium sulphate and then concentrated on a rotary evaporator. Approx. 77 g of a crude product were thus obtained, which was used thus in the next stage.

1. additionwere added dropwise within 1 h
2. waitThe mixture was left
3. waitSubsequently, at −72° C., within 2 h
4. waitleft
5. stirringto stir at this temperature for 1 h
6. customthe phases were separated
7. extractionthe aqueous phase was re-extracted twice with a further 100 ml of toluene
8. dry with materialThe combined organic phases were dried over sodium sulphate
9. concentrationconcentrated on a rotary evaporator

ORD record

ord-51579771ed8441fd9429705ab154bba6

Source dataset

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08063226B2