HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → 1,1-Dichloroethane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 2-Methylbenzenesulfonic acid | HCID 6925 | — |
| Reactant | Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)- | HCID 18462 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | 1,1-Dichloroethane | HCID 6365 | — |
| Product | Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)- | HCID 18462 | — |
Reaction Steps
Compound 2 is first treated as described above in Method B, Step 1, to obtain an intermediate phenol dihydropyridine which is then treated with about 0.1-0.3 meq (preferably 0.1 meq) of an acid (toluenesulfonic acid, camphorsulfonic acid, trifluoroacetic acid, methanesulfonic acid, sulfuric acid; preferably, camphorsulfonic acid) in a solvent such as CH2Cl2, CHCl3, dichloroethane, THF, DME, or mixtures thereof (preferably methylene chloride) at about 25° to 50° C. for about 2-24 hours to obtain compound 1a.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04579851 |
| Source dataset | uspto-grants-1986_04 |
| ORD ID | ord-21e540b526814508b26cee12aff2f2ed |
| Source note | uspto-grants-1986_04 |