Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloroacetyl chloride | HCID 6593 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 57526993 | HCID 57526993 | 92.5% |
Reaction Steps
N,O-Dimethylhydroxylamine hydrochloride (7.94 g, 81.4 mmol) and K2CO3 (17.2 g, 124.1 mmol) were added to a water (70 ml) and toluene (70 ml) mixture. The mixture was then cooled to 0° C. Dichloroacetyl chloride (10 g, 67.85 mmol) was added drop wise and the reaction was allowed to warm to room temperature overnight. The toluene was collected and then the aqueous layer was extracted with EtOAc (2×100 ml). The organic layers were dried over sodium sulfate and concentrated in vacuo to give the title product (10.8 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07473699B2 |
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| Source dataset | uspto-grants-2009_01 |
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| ORD ID | ord-b595e9f5b3624abbb987f3ade259afd8 |
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| Source note | uspto-grants-2009_01 |
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