Water → HCID 86703815, compound

To an ice/water bath cooled flask containing a solution of 6-mercaptohexanoic acid (500.0 mg, 3.37 mmol) de ionized water (2 mL) was added a solution of S-Methyl methanethiosulfonate (468 mg, 3.71 mmol) in ethanol (1 mL). After 16 hr the reaction was diluted with saturated sodium chloride (400 mL) and extracted with ethyl ether (3×150 mL). The combined extracts were washed with saturated NaCl (100 mL), dried over anhydrous Na2SO4 and concentrated in vacuo. The product was purified by silica chromatography eluting with ethyl acetate/hexanes/acetic acid (40:58:2). Product containing fractions were combined and concentrated in vacuo to give 482 mg (73% yield) of the desired product. MS calcd (M+Na)+, 217.3; found, 217.3

1. temperatureTo an ice/water bath cooled flask
2. extractionextracted with ethyl ether (3×150 mL)
3. washThe combined extracts were washed with saturated NaCl (100 mL)
4. dry with materialdried over anhydrous Na2SO4
5. concentrationconcentrated in vacuo
6. customThe product was purified by silica chromatography
7. washeluting with ethyl acetate/hexanes/acetic acid (40:58:2)
8. additionProduct containing fractions
9. concentrationconcentrated in vacuo

ORD record

ord-5f20726fb1f3452dbb99f18eb06e4e2c

Source dataset

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09090629B2