Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Trimethyl orthoacetate | HCID 15050 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 59472955 | HCID 59472955 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 59472976 | HCID 59472976 | — |
Reaction Steps
To a stirred solution of 16-2 (5 g, 11.3 mMol) in 20 mL of 3:1 toluene:methanol was added trimethyl orthoacetate (1.8 g, 15.3 mMol) and p-toluenesulfonic acid monohydrate (0.1 g, 0.6 mMol). The reaction was heated to 100° C. in a microwave reactor for 35 minutes. After cooling to room temperature, the solvent was removed under reduced pressure. The residue was purified using normal phase flash chromatography to yield 17-1 as a solid. LC/MS (M+1) calculated: 466.6 observed: 466.2
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08008317B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-d730916fbeac4586b21f2e84e0ad3423 |
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| Source note | uspto-grants-2011_08 |
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