HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 59135975, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 59136018 | HCID 59136018 | — |
| Reactant | HCID 178467906 | HCID 178467906 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59135975 | HCID 59135975 | 44% |
Reaction Steps
To a solution of methyl (2-{7-[methyl(2-thienylsulfonyl)amino]-1H-indol-2-yl}-1-thia-3,8-diazaspiro[4.5]dec-2-en-8-yl)acetate (211 mg) in tetrahydrofuran (3 mL) was added 1.5M methyllithium-diethyl ether solution (2 mL) at room temperature, and the mixture was stirred for 30 min. Saturated aqueous ammonium chloride solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4), and concentrated. The obtained residue was subjected to silica gel column chromatography to give the title compound (92 mg, yield 44%) as white crystals from a fraction eluted with ethyl acetate:hexane=1:3. melting point 191° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07777047B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-19bc726b67aa4c639ed7bfbcd935d541 |
| Source note | uspto-grants-2010_08 |