HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 178505100, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 178510990 | HCID 178510990 | — |
| Product | HCID 178505100 | HCID 178505100 | — |
Reaction Steps
Methanesulfonyl chloride (0.019 mL, 0.245 mmole) was added dropwise to a solution of 8-{3-[(6-aminohexyl)oxy]benzyl}-4-(cyclohexylamino)-1-(3-fluorophenyl)-1,3,8-triazaspiro[4.5]dec-3-en-2-one (0.116 mg, 0.222 mmole) in 5 mL CH2Cl2 at rt, and Et3N (0.034 mL, 0.245 mmole. After stirring for 0.5 hr at rt, the reaction was concentrated in vacuo. The residue was redissolved in CH2Cl2, washed with H2O, and then brine. Dried over Na2SO4, filtered and conc in vacuo. The residue was purified on a 40 g silica gel column eluting with 100% CH2Cl2 saturated with ammonia to 4% MeOH in CH2Cl2 saturated with ammonia. The clean fractions were combined and concentrated in vacuo to yield the product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08114887B2 |
| Source dataset | uspto-grants-2012_02 |
| ORD ID | ord-3f9b12352a9a48cdb56054eb4fec9e59 |
| Source note | uspto-grants-2012_02 |