HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178501242, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Methylpropane-2-sulfinyl chloride | HCID 4686861 | — |
| Reactant | HCID 178501209 | HCID 178501209 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178501242 | HCID 178501242 | 109.2% |
Reaction Steps
Triethylamine (272 mL) was added dropwise to a suspension of methyl cis-4-amino-1-cyclohexane carboxylate hydrochloride (7) (151 g, 0.78 mol) and 2-methylpropane-2-sulfinyl chloride (3) (120.8 g, 1.1 eq) in ethyl acetate (755 mL) at 6 to 9° C. The mixture was stirred for an hour at the same temperature and poured into diluted hydrochloric acid. The mixture was extracted with ethyl acetate (750 mL×2) and each of organic layers was washed with water, 5% aqueous solution of sodium bicarbonate, water and brine, successively. The solvent was concentrated under reduced pressure to obtain oily (14) (222.7 g, 109%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07459580B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-34b83c1e2fef4acba225753dc8ad2772 |
| Source note | uspto-grants-2008_12 |