HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 68506957, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 86645307 | HCID 86645307 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68506957 | HCID 68506957 | 58.9% |
Reaction Steps
To a solution of Intermediate 12 (100 mg, 0.28 mmol) and DIPEA (97 μL, 0.57 mmol) in DCM (2 mL) at 0° C. is added dropwise a solution of methanesulfonyl chloride (33 μL, 0.43 mmol) in DCM (2 mL). The reaction mixture is stirred at rt for 1 h and is then diluted with EtOAc, and washed with sat. aq. NaHCO3. The org. phase is dried over MgSO4, filtered, evaporated and purified by prep. TLC (eluting with Heptane/EtOAc 1:1) to give the title compound (71 mg) as a yellow solid; LC-MS: tR=1.07 min; [M+H]+=431.07.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08299086B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-6b08d99c98d84ba893efabae1d0d7f6c |
| Source note | uspto-grants-2012_10 |