HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178426465, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 178426466 | HCID 178426466 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178426465 | HCID 178426465 | 108% |
Reaction Steps
A solution of 0.246 g (0.95 mmol) of trans-3-{4-[Methyl-(6-methyl-pyridazin-3-yl)-amino]-cyclohexyl}-prop-2-yn-1-ol in 7 ml CH2Cl2 was treated at 0° C. with 0.081 ml (1.04 mmol) methanesulfonylchloride and 0.17 ml (1.42 mmol) 2,6-lutidine. The reaction was stirred for 22 h at room temperature, water (1 ml) was added and stirred for 5 min. After extraction with aqueous saturated NaHCO3/Et2O(3×), the organic phase was washed with aqueous 10% NaCl, dried over Na2SO4 and evaporated to yield 0.285 g of crude trans-[4-(3-Chloro-prop-1-ynyl)-cyclohexyl]-methyl-(6-methyl-pyridazin-3-yl)-amine, MS: 278 (MH+, 1Cl).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07012077B2 |
| Source dataset | uspto-grants-2006_03 |
| ORD ID | ord-87c748018a5c499ead27ada14a3c9ec5 |
| Source note | uspto-grants-2006_03 |