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 at the same temperature range until the reaction was complete. After that time, the solution turned into a suspension. The suspension formed was filtered and the solid was washed with chlorobenzene (50 ml). The filtrate was washed with water (3×225 mL). The resulting organic phase was dried with 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. customThe suspension formed
3. filtrationwas filtered
4. washthe solid was 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 magnesium sulfate
7. concentrationconcentrated
8. distillationThe crude product was purified by distillation

ORDレコード

ord-ac6abd8c8aa745709b6510de5fb3e91a

出典データセット

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09290446B2