Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | HCID 70104303 | HCID 70104303 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 70103189 | HCID 70103189 | — |
Reaction Steps
7.94 g of the product obtained in Stage C above is introduced at ambient temperature into 80 cm3 of anhydrous THF, followed by cooling down to -78° C. and 13.75 cm3 of a 1.6M n-butyllithium solution in hexane is added. After 10 minutes, 15 cm3 of ethyl chloroformate is added, followed by agitation for another 15 minutes at -78° C. 60 cm3 of water is added, the reaction medium is left to return to ambient temperature, the THF is evaporated off, 10 cm3 of 32% soda is added to destroy the excess ethyl chloroformate, followed by extraction with 3×200 cm3 of AcOEt, washing with 2×80 cm3 of water, drying, filtering and evaporating.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05807878 |
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| Source dataset | uspto-grants-1998_09 |
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| ORD ID | ord-293a73684e7d4982a53335e6257874c7 |
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| Source note | uspto-grants-1998_09 |
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