HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 46832634, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 58074628 | HCID 58074628 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 46832634 | HCID 46832634 | — |
Reaction Steps
Compound 248 (0.02 g, 0.06 mmol) was dissolved in DCM (2 mL). TEA (0.035 mL, 0.25 mmol) and methanesulfonyl chloride (0.007 mL, 0.09 mmol) were added and stirred under argon for 30 min. The reaction mixture was washed with H2O and the organic phase was filtered through a phase separation cartridge (chromabond PTS). The solvent was concentrated and the crude product was suspended in iso-butanol (6 mL) under an argon atmosphere. DIPEA (0.05 mL, 0.31 mmol) was added and the mixture was stirred at 60° C. for 18 h. Iso-butanol was evaporated and the crude product was purified by preparative HPLC/MS to afford the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08952162B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-cead62b2328b4a0e880f3ba993b889fa |
| Source note | uspto-grants-2015_02 |