HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13151172, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Pyrrolidone | HCID 12025 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 13222926 | HCID 13222926 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 13151172 | HCID 13151172 | — |
Reaction Steps
6-Carbomethoxy-3,4-dihydro-2,2-dimethyl-3,4-epoxy-2H-benzo[b]pyran (2.42 g, the preparation of which is described in Example 4 of U.K. Pat. No. 1,511,187) and 2-pyrrolidone (0.88 g), were stirred in dimethyl sulphoxide (40 ml) under nitrogen at room temperature. Sodium hydride (0.31 g, 81% dispersion in mineral oil) was added during 5 mins. and the reaction stirred for a further 6 hours. Addition of water, extraction with ethyl acetate, drying or the organic phase with magnesium sulphate, filtration, evaporation and recrystallisation from ethyl acetate-pentane gave 6-carbomethoxy-3,4-dihydro-2,2-dimethyl-trans-4-(2-oxo-1-pyrrolidinyl)-2H-benzo[b]-pyran-3-ol of m.p. 190°-192°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04446113 |
| Source dataset | uspto-grants-1984_05 |
| ORD ID | ord-ca24158647394ce88990a27f5fd71449 |
| Source note | uspto-grants-1984_05 |