HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 178515732, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium ethanethiol | HCID 45051917 | — |
| Reactant | HCID 178490244 | HCID 178490244 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178515732 | HCID 178515732 | 63.2% |
Reaction Steps
Dissolve 3-(2-chloro-6-methoxy-benzyl)-1-(cis-4-hydroxy-cyclohexyl)-pyrrolidin-2-one (Example 57) (150 mg, 0.44 mmol) in DMF (5 mL) and purge with nitrogen. Add sodium ethane thiol (110 mg, 1.3 mmol) and heat to 120° C. for 4 hours. Cool to room temperature and pour into ammonium chloride and extract with methylene chloride, dry over sodium sulfate, filter and concentrate. Purify over silica gel (20% hexanes in ethyl acetate) to yield 90 mg (63%) of the title compound as a pale yellow solid: Mass spectrum (apci) m/z=324.1 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07713979B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-36054c0778964a35ad1bf6966c61ee27 |
| Source note | uspto-grants-2010_05 |