HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Disulfide → HCID 59424691, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Disulfide | HCID 12232 | — |
| Reactant | 7-Chlorothieno[3,2-b]pyridine | HCID 11275251 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59424691 | HCID 59424691 | 94.3% |
Reaction Steps
To a solution of 2 (200 mg, 1.18 mmol) in dry THF (11 ml) at −78° C. was added n-BuLi (0.57 mL, 2.5M solution on hexane, 1.41 mmol) and the resultant brown precipitate was stirred for 10 minutes. Methyl disulfide (0.16 ml, 1.77 mmol) was added slowly, the mixture was stirred at −78° C. for 3 hours and partitioned between DCM and water. Organic phase was separated, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to afford title compound 229 (0.240 g, 94% yield, crude) as a yellow solid. MS (m/z): 216.1 (100%), 218.1 (39%) (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07772247B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-281d2ebb2ff840bb821eeb1a45aa8359 |
| Source note | uspto-grants-2010_08 |