Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroacetone | HCID 6571 | — |
| Reactant | HCID 86650781 | HCID 86650781 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58135242 | HCID 58135242 | — |
Reaction Steps
The compound (0.70 g, 2.1 mmol) obtained in step A was dissolved in a ethanol (14 ml)-N,N-dimethylformamide (4 ml) mixed solvent. Then, chloroacetone (0.18 ml, 2.3 mmol) was added, and the mixture was stirred at 80° C. for 3 hr. The reaction mixture was concentrated under reduced pressure, and the obtained oil was diluted with dichloromethane, washed with water, saturated aqueous sodium hydrogen carbonate and saturated brine, and dried over anhydrous magnesium sulfate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure to give a crude oil of the title compound containing N,N-dimethylformamide. Using this oil and according to the method of Reference Example 62, step B, the title compound (0.56 g, yield 83%) was obtained as a pale-yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08513235B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-b9ea0110e6c24b8e906d55f58cc81d57 |
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| Source note | uspto-grants-2013_08 |
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