HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Thiosulfate → 4-(2,5,5-Trimethyl-[1,3]dioxan-2-yl)-cyclohexanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Methyl morpholine oxide | HCID 82029 | — |
| Reactant | 4-(2,5,5-Trimethyl-[1,3]dioxan-2-yl)-cyclohexanol | HCID 23147957 | — |
| Catalyst | HCID 178419074 | HCID 178419074 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 4-(2,5,5-Trimethyl-[1,3]dioxan-2-yl)-cyclohexanone | HCID 23147947 | 85% |
Reaction Steps
TPAP (161 mg, 0.05 eq.) was added to a solution of 4-(2,5,5-trimethyl-[1,3]dioxan-2-yl)-cyclohexanol (2.22 g, 1 eq.) and NMO (2.28 g, 2 eq.) in MeCN (65 mL). The reaction mixture was stirred at room temperature overnight. Saturated aqueous solution of Na2S2O3 was added to the mixture and the resulting mixture was stirred vigorously for 15 minutes. The separated aqueous phase was extracted with CH2Cl2. The combined organic layer was dried over Na2SO4, filtered through Celite and concentrated. The crude product was purified by silica gel column chromatography (25% to 50% EtOAc/hexanes) to give 4-(2,5,5-trimethyl-[1,3]dioxan-2-yl)-cyclohexanone (1.87 g, 85%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07868002B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-c847e169d6cd4642871842fcc15b9c0a |
| Source note | uspto-grants-2011_01 |