Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dibah | HCID 16682954 | — |
| Reactant | HCID 86708071 | HCID 86708071 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 86708072 | HCID 86708072 | 100% |
Reaction Steps
To a solution of the material from Step 2 (9.73 g, 24.12 mmol) in diethyl ether (240 mL) at −70° C. was slowly added 1.0 M Dibal-H (40.2 mL, 40.2 mmol) in toluene. The reaction mixture was stirred at −70° C. for 45 minutes. Water (10 mL) was slowly added, and the reaction mixture was allowed to warm up to room temperature and aged for 30 minutes. Additional water (80 mL) was added, and aged for 1 hour. It was filtered on a short pad of celite, rinsed with tert-butyl methyl ether (3×). The filtrate was washed with brine, dried over MgSO4, filtered and concentrated in vacuo to afford 8.67 g of the title compound that was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09079834B2 |
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| Source dataset | uspto-grants-2015_07 |
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| ORD ID | ord-1ea36e859747435f806eb68a2f5c6b9d |
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| Source note | uspto-grants-2015_07 |
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