HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → (3aR,5R,6R,7R,7aR)-5-(acetoxymethyl)-2-methyl-5,6,7,7a-tetrahydro-3aH-pyrano[3,2-d]oxazole-6,7-diyl diacetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trimethylsilyl triflate | HCID 65367 | — |
| Reactant | beta-D-Galactopyranose, 2-(acetylamino)-2-deoxy-, 1,3,4,6-tetraacetate | HCID 6547253 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (3aR,5R,6R,7R,7aR)-5-(acetoxymethyl)-2-methyl-5,6,7,7a-tetrahydro-3aH-pyrano[3,2-d]oxazole-6,7-diyl diacetate | HCID 11278902 | 120.3% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
Commercially available acetic acid (2S,3R,4R,5R,6R)-4,5-diacetoxy-6-acetoxymethyl-3-acetylamino-tetrahydro-pyran-2-yl ester (10.0 g, 26 mmol) was dissolved in 116 mL of abs. CH2Cl2 and treated with trimethylsilyl triflate (14.27 g, 64 mmol). The reaction was allowed to proceed over night at 45° C. After cooling to 0° C., triethylamine (4.88 ml, 35 mmol) was added, the mixture diluted with CH2Cl2 and washed with NaHCO3-solution and water. Drying over Na2SO4 and evaporation of the solvent yielded 10.3 g of the title compound as brownish oil which was used without further purification for the next step. MS (ISP): 330.0 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09345775B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-c23fb3e8500a481e8b75210f8bc82cc5 |
| Source note | uspto-grants-2016_05 |