HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178482151, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 178482150 | HCID 178482150 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178482151 | HCID 178482151 | 106% |
Reaction Steps
A solution of 1.08 g (3.68 mmol) of trans-4-{4-[(6-Chloro-pyridazin-3-yl)-methyl-amino]-cyclohexyl}-but-2-yn-1-ol in 30 ml CH2Cl2 was treated at 0° C. with 0.31 ml (4.04 mmol) methanesulfonylchloride and 0.64 ml (5.51 mmol) 2,6-lutidine. The reaction was stirred for 46 h at room temperature, water (4 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 1.45 g of crude trans-Methanesulfonic acid 4-{4-[(6-chloro-pyridazin-3-yl)-methyl-amino]-cyclohexyl}-but-2-ynyl ester, MS: 372 (MH+, 1Cl).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07012077B2 |
| Source dataset | uspto-grants-2006_03 |
| ORD ID | ord-98ac12727cca4176a09373bfee0f60ac |
| Source note | uspto-grants-2006_03 |