HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 178505325, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 178526785 | HCID 178526785 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178505325 | HCID 178505325 | 90% |
Reaction Steps
To a mixture of trans-4-[(6-nitrothieno[3,2-b]pyridin-7-yl)amino]cyclohexanol (0.21 g, 0.72 mmol) (Example 3, Step 1) and N,N-diisopropylethylamine (0.25 mL, 1.4 mmol) in methylene chloride (2 mL) was added methanesulfonyl chloride (0.083 mL, 1.1 mmol). The reaction was stirred at room temperature for 2 h. After dilution with sat. aq. NaHCO3 solution, the resulting mixture was extracted with dichloromethane. The organic layers were concentrated and purified on silica gel (eluting with 0 to 5% MeOH in dichloromethane) to give the desired product (0.24 g, 90%). LCMS calculated for C14H18N3O5S2 (M+H)+: m/z=372.1. Found: 372.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181271B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-b9ed7ef903f44d10b0b634779509d5de |
| Source note | uspto-grants-2015_11 |