HuagongsheHuagongshe Chemistry Print Report · For research reference only
Solketal → HCID 86612334, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Solketal | HCID 7528 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Di(succinimido) carbonate | HCID 676246 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86612334 | HCID 86612334 | 122% |
Reaction Steps
To a solution of (2,2-dimethyl-[1,3]dioxolan-4-yl)-methanol (0.4 g, 3.0 mmol) in acetonitrile (10 mL) was added carbonic acid bis-(2,5-dioxo-pyrrolidin-1-yl) ester (1.15 g, 4.5 mmol) and triethylamine (0.84 mL, 6.0 mmol). After stirring at ambient temperature for 10 min, the mixture was concentrated at reduced pressure, sat. NaHCO3 (50 mL)was added, and the solution was extracted with ethyl acetate and organic phase was separated and concentrated to obtain 1.0 g of crude product that was used without further purification in the next step. MS (APCI) m/z: 273 [M+H]+ 1H NMR (DMSO-d6) δ: 4.50 (m, 1H), 4.40-4.29 (m, 2H), 4.04 (m, 1H), 3.73 (dd, J=6.0 and 9.0 Hz, 1H), 2.80 (s, 4H), 1.35 (s, 3H), 1.30 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08232309B2 |
| Source dataset | uspto-grants-2012_07 |
| ORD ID | ord-4de78232db5147a796b5e8b540a51478 |
| Source note | uspto-grants-2012_07 |