Chlorosuccinimide → Chloromethyl p-Tolyl Sulfide

Methyl p-tolyl sulfide (75 g, 542.27 mmol) was diluted in chorobenzene (452 mL). N-Chloro Succinimide (NCS) (76.07 g, 1.05 eq) was added in small portions maintaining the temperature between 35° C. and 45° C., under an argon atmosphere. The reaction mixture was stirred within the same temperature range until the reaction was complete. Thereafter, a solid separated out from the solution. The suspension was filtered, and the solid washed with chlorobenzene (50 ml). The filtrate was washed with water (3×225 mL). The resulting organic phase was dried with anhydrous magnesium sulfate and concentrated. The crude product was purified by distillation to give 102.68 g (100%) of the desired product as yellow oil (bp: 96° C. at 40 Pa).

1. temperaturemaintaining the temperature between 35° C. and 45° C.
2. customThereafter, a solid separated out from the solution
3. filtrationThe suspension was filtered
4. washthe solid washed with chlorobenzene (50 ml)
5. washThe filtrate was washed with water (3×225 mL)
6. dry with materialThe resulting organic phase was dried with anhydrous magnesium sulfate
7. concentrationconcentrated
8. distillationThe crude product was purified by distillation

ORDレコード

ord-64d0d56ed88948098b1ece6479b3b27b

出典データセット

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09290446B2