HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2-Dimethyl-1,3-dioxane-4,6-dione → HCID 58392263, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2-Dimethyl-1,3-dioxane-4,6-dione | HCID 16249 | — |
| Reactant | 4-Chloro-2-fluorobenzaldehyde | HCID 2724908 | — |
| Reactant | 5-Fluoro-7-[(methylsulfanyl)methyl]-1H-indole | HCID 58392227 | — |
| Catalyst | proline dl-form | HCID 614 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 58392263 | HCID 58392263 | 103.9% |
Reaction Steps
0.70 g (4.41 mmol) of 4-chloro-2-fluorobenzaldehyde, 0.64 g (4.41 mmol) of Meldrum's acid and 24 mg (0.21 mmol) of D,L-proline were added to a solution of 1.00 g of the compound of Example 11A with a purity of 82% (4.20 mmol) in 35 ml of acetonitrile. The reaction mixture was stirred at RT overnight. It was concentrated, and the residue was taken up in ethyl acetate, washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution and water, dried over magnesium sulfate, filtered and concentrated. 2.20 g of the title compound were obtained with a purity of 71% (78% of theory) and were reacted without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063234B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-26431e6a4a6c4a25a011ddb335f4ea16 |
| Source note | uspto-grants-2011_11 |