Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 19041800 | HCID 19041800 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19041797 | HCID 19041797 | — |
Reaction Steps
Lithium aluminum hydride (0.553 g, 14.58 mmole) is added to 10 ml dry diethyl ether and 10 ml dry THF. To this slurry is added dropwise 4-(3,5-dimethoxy-4-hydroxyphenyl)-1,3-dithiolane-2-thione (34) (2.00 g, 6.94 mmole) predissolved in 40 ml dry THF. The reaction is stirred under a nitrogen (N2) atmosphere until the solution becomes colorless (1 hour). The reaction is cooled to 0° C. and the excess hydride destroyed with H2O. The reaction mixture is acidified with 10% HCl and immediately extracted with diethyl ether. The organic layer was washed with H2O, dried over MgSO4, filtered and evaporated to a white solid (1.64 g, 96%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05639782 |
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| Source dataset | uspto-grants-1997_06 |
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| ORD ID | ord-fa32af613c2c4e839fe4ed7a69139b60 |
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| Source note | uspto-grants-1997_06 |
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