Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Glycerol | HCID 753 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 1,3-Benzodioxole, 5-nitro- | HCID 75798 | — |
| Product | HCID 20074437 | HCID 20074437 | — |
Reaction Steps
0.3 mol (19.8 g) of 85% by weight potassium hydroxide pellets is dissolved in 210 ml of glycerol, and 0.25 mol (41.75 g) of 3,4-methylenedioxynitrobenzene is then added, with stirring. After heating for one and a half hours in the region of 110° C., the reaction medium is poured into 1.5 litres of iced water. The mixture is filtered in order to remove a small quantity of starting material. The filtrate is acidified to pH=4 with hydrochloric acid and then treated with 10 g of vegetable charcoal. After stirring for a few minutes at ambient temperature and removal of the vegetable charcoal by filtration, the solution is left to stand overnight at 0° C. and the expected product which has crystallized is then filtered off. After recrystallization from ethanol and drying in vacuo, the product melts at 148° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04954131 |
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| Source dataset | uspto-grants-1990_09 |
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| ORD ID | ord-4503d509850c45ff894fa9e1c5ff28b8 |
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| Source note | uspto-grants-1990_09 |
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