反应详情

Stir a mixture of heptanes (1.5 L), methanol (0.4 L), and 1-(4-chloro-2-fluorophenyl)ethanone (1 kg, 5.81 mol) with cooling to <5° C. Add sulfuryl chloride (0.608 L, 1.02 kg, 7.55 mol) as a heptanes (1.5 L) solution drop-wise to the mixture keeping the reaction temperature <15° C. during the addition. After 2 h quench the reaction at ambient temperature to a pH of 6 with sodium hydroxide (5N, 2.0 L). Extract the reaction mixture with methylene chloride (2 L) and concentrate the extract to form a white solid. Filter and dry the solid.

1. temperaturewith cooling to <5° C
2. customthe reaction temperature <15° C.
3. additionduring the addition
4. customAfter 2 h quench
5. customthe reaction at ambient temperature to a pH of 6 with sodium hydroxide (5N, 2.0 L)
6. extractionExtract the reaction mixture with methylene chloride (2 L)
7. concentrationconcentrate the
8. extractionextract
9. customto form a white solid
10. filtrationFilter
11. customdry the solid