Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Trifluoromethanesulfonic acid | HCID 62406 | — |
| Reactant | Benzyl 2,2,2-trichloroacetimidate | HCID 144968 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 18369547 | HCID 18369547 | 70% |
Reaction Steps
A diethyl ether solution of 260 mg of 2,2,2-trichloro-1-(phenylmethoxy)ethanimine synthesized in the production example 30 was added to 4 ml of a diethyl ether solution of the compound obtained in the production example 29 to prepare the homogeneous solution, and the flask was immersed in an ice water bath. The solution in the flask was mixed with 10 μl of trifluoromethanesulfonic acid, gradually heated up to room temperature, and simultaneously stirred for 17 hours. After the reaction was finished, the reaction solution was diluted with ethyl acetate and extracted. The obtained organic layers were integrated, sequentially washed with a saturated aqueous solution of sodium bicarbonate and with a saturated aqueous solution of sodium chloride, and then dried over Na2SO4. The solvent was distilled away under reduced pressure, and the residue was purified by column chromatography to obtain the title compound (120 mg, 70%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06348478B1 |
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| Source dataset | uspto-grants-2002_02 |
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| ORD ID | ord-6ebdff1cdfdc4291a19d384ddf54a393 |
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| Source note | uspto-grants-2002_02 |
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