HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178483660, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 178483648 | HCID 178483648 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178483660 | HCID 178483660 | 98.3% |
Reaction Steps
To an ice-cooled solution of 10 g (36.8 mmol) of trans-[2-(4-hydroxymethyl-cyclohexyl)-ethyl]-methyl-carbamic acid tert-butyl ester in 100 mL of CH2Cl2 were added 3.15 mL (40.5 mmol, 1.3 eq) of methanesulfonyl chloride followed by 6.68 mL (47.9 mmol, 1.3 eq) of triethylamine. Then the reaction mixture was stirred at RT for 1 h. 1M HCl was added, the phases were separated and the inorganic phase was washed with ether. The combined organic phases were washed with water and dried over magnesium sulfate. Concentration of the solution yielded 12.64 g (98%) of trans-methanesulfonic acid 4-[2-(tert-butoxycarbonyl-methyl-amino)-ethyl]-cyclohexylmethyl ester as colorless oil, MS: 367 (M+NH4+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06965048B2 |
| Source dataset | uspto-grants-2005_11 |
| ORD ID | ord-d029d62cae7147b49b29ed64a1ce55e0 |
| Source note | uspto-grants-2005_11 |