Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Bisulfate | HCID 516919 | — |
| Reactant | HCID 18619999 | HCID 18619999 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69885714 | HCID 69885714 | 78% |
Reaction Steps
In 20 ml of dichloromethane, was dissolved 298 mg of the compound obtained in Example 16. To the resulting solution, was added 3.0 ml of triethylamine. To the obtained mixture, 0.46 ml of acetyl chloride was added under cooling with ice and stirring. The mixture was stirred at 0° C. to room temperature for 18 hours. The obtained mixture was poured into a saturated aqueous solution of sodium hydrogensulfate and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate and saturated brine and subsequently dried over magnesium sulfate. The solvent was removed under reduced pressure, and the obtained crude product was purified by silica gel column chromatography to afford 260 mg (78%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06538137B1 |
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| Source dataset | uspto-grants-2003_03 |
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| ORD ID | ord-9827e698158e4b75b93af5afaa40d021 |
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| Source note | uspto-grants-2003_03 |
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