Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | tert-Butanol | HCID 6386 | — |
| Reactant | HCID 68004032 | HCID 68004032 | — |
| Product | HCID 86684752 | HCID 86684752 | 97% |
Reaction Steps
To a solution of 24 (1.60 g, 4.7 mmol) in t-butanol (20 mL) and H2O (20 mL) AD-mix-beta (5.0 g) was added portion wise at 5° C. The reaction was slowly warmed to room temperature and further stirred at this temperature for 16 hrs. The reaction mixture was cooled down to 5° C. and then quenched by adding excess sodium sulfite and stirred for 20 min. The resulting mixture was diluted with water (100 mL) and extracted with ethyl acetate (100 mL×2). The organic layers were combined which was washed with brine, dried over Na2SO4, and concentrated. The obtained residue was and chromatographed on silica gel eluted with hexane/ethyl acetate (20%-100%) to afford 1.70 g (97%) of 25 as a colorless oil which was use directly for the next step. LC/Ms (M+1) 373.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08921373B2 |
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| Source dataset | uspto-grants-2014_12 |
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| ORD ID | ord-ffda992d10f6465fabebebe56085c085 |
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| Source note | uspto-grants-2014_12 |
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