Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | 2-Methyl-propane-2-sulfinic acid 1-[4-(tert-butyl-dimethyl-silanyloxy)-1-trifluoromethyl-cyclohexyl]-methylideneamide | HCID 67072797 | — |
| Reactant | HCID 178461633 | HCID 178461633 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 67072554 | HCID 67072554 | — |
Reaction Steps
13.4 ml (26.8 mmol) of a 2M solution of ethylmagnesium chloride in diethyl ether were diluted using 8 ml of anhydrous diethyl ether and cooled to −78° C. At that temperature, a solution of 3.7 g (8.95 mmol) of 2-methyl-propane-2-sulfinic acid 1-[4-(tert-butyl-dimethyl-silanyloxy)-1-trifluoromethyl-cyclohexyl]methylideneamide (72) in anhydrous diethyl ether was added dropwise. Afterwards, the mixture was allowed to warm to ambient temperature and was stirred for 2 h at ambient temperature. 100 ml of a saturated aqueous Na2SO4-solution was added, the organic layer separated, dried using MgSO4 and evaporated to give 3.22 g of 73 as an oil, used without further purification. Rt=1.09 min (Method Q).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08399482B2 |
|---|
| Source dataset | uspto-grants-2013_03 |
|---|
| ORD ID | ord-7b62317794e040aba0dd881ab6efabcb |
|---|
| Source note | uspto-grants-2013_03 |
|---|