HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium methanethiolate → HCID 68687732, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium methanethiolate | HCID 4378561 | — |
| Reactant | HCID 16115648 | HCID 16115648 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68687732 | HCID 68687732 | 65% |
Reaction Steps
To a stirring solution of N-(t-butoxycarbonyl)-(R)-1,3,4,10b-tetrahydro-9-bromo-7-trifluoromethyl-pyrazino[2,1-a]isoindol-6(2H)-one (56 mg, 0.13 mmol) in dry DMF (1 mL) at 60° C. was added sodium methanethiolate (9.9 mg, 0.14 mmol). The reaction was heated to reflux for 30 min and then cooled to room temperature. The reaction was quenched with 1M aq. NaOH and extracted with EtOAc (3×5 mL). The organic layers were combined, dried over Na2SO4, and conc. in vacuo to a yellow oil. The oil was purified by flash chromatography (silica gel, 0–33% EtOAc in hexanes) to give 34 mg of the desired product as a colorless oil. MS (ESI) 403 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07244843B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-5b0592bf5ce245cba53c5981ed4068b3 |
| Source note | uspto-grants-2007_07 |