Hydrochloric Acid → 2-Mercapto-5-methyl-4-heptanone

Temperature

40 °C

A reaction flask was charged with HCl (1.25 M, 500 mL) in methanol (0.63 mol). S-(5-methyl-4-oxoheptan-2-yl) ethanethioate (127.0 g, 0.63 mol) (synthesized as above in EXAMPLE I) then added into the reaction flask in one portion. The reaction mixture was stirred at 40° C. for about 48 hours, then cooled down to room temperature, and transferred into a separatory funnel Water (250 mL) was added. The reaction mixture was then extracted twice with ethyl acetate (250 mL each time). The organic phases were combined, washed with water (250 mL) followed by brine (100 mL), and then dried with magnesium sulfate. Further distillation of the obtained crude product under a vacuum (at 57° C. with a pressure of 1.33 mmHg) provided 2-mercapto-5-methyl-heptan-4-one (76.0 g) (about 76% yield with a purity over 98% monitored with gas chromatography).

1. temperaturecooled down to room temperature
2. customtransferred into a separatory funnel
3. extractionThe reaction mixture was then extracted twice with ethyl acetate (250 mL each time)
4. washwashed with water (250 mL)
5. dry with materialdried with magnesium sulfate
6. distillationFurther distillation of the
7. customobtained crude product under a vacuum (at 57° C. with a pressure of 1.33 mmHg)

ORD record

ord-01fc8538e7174ff1b66bbea7837ce64e

Source dataset

uspto-grants-2015_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09179701B2