Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 24814177 | HCID 24814177 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 24814178 | HCID 24814178 | 97% |
Reaction Steps
A solution of compound 7 (1.35 g, 3 mmol) in 20 mL of THF is added dropwise to a suspension of lithium aluminium hydride (LiAlH4, 1.7 g, 45 mmol, 15 eq.) in dry tetrahydrofuran (THF) (30 mL) at −78° C. The temperature of the medium is allowed to return to room temperature and then the reaction is heated under reflux with stirring. After 1 hour, the solution is cooled to −78° C. and diluted with dichloromethane, and then water (10 mL) is slowly poured in. The solid obtained is filtered and washed with dichloromethane. The mother liquors are washed with water and with brine and then dried and concentrated to give 1.05 g (2.88 mmol) of a pasty compound (yield: 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08664400B2 |
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| Source dataset | uspto-grants-2014_03 |
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| ORD ID | ord-1a5a14bbd1f84301815b922e4b4f665f |
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| Source note | uspto-grants-2014_03 |
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