Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 20083162 | HCID 20083162 | — |
| Product | HCID 20083173 | HCID 20083173 | 57.3% |
Reaction Steps
To 1.45 g (4.7 mmol) of the compound (155) obtained in Example 33, 10 ml (109 mmol) of dimethyl sulfate was added, and the solution was heated 3.5 hours at 120° C. After air-cooling, to 90 ml of ice/water containing 15 g (109 mmol) of anhydrous potassium carbonate, the solution was added, and the solution was stirred overnight. The solution was extracted with 50 ml of chloroform, and after drying over magnesium sulfate, the solvent was removed by distillation. The residue was separated by column chromatography (silica gel 8 g, eluent solvent; chloroform:methanol=100:1) to obtain 830 mg of the subject compound (156) in a 57% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05254685 |
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| Source dataset | uspto-grants-1993_10 |
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| ORD ID | ord-6954046db06d419dbda06c8aaaf649da |
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| Source note | uspto-grants-1993_10 |
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