Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | HCID 86623036 | HCID 86623036 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86623037 | HCID 86623037 | 98% |
Reaction Steps
The Boc-aminopropanol-fenbufen obtained above (1.82 mmol) was dissolved in dichloromethane (4 ml), and under ice-cooling, 4 N hydrochloric acid ethyl acetate solution (4 ml) was added thereto, and then the mixture was gradually returned to room temperature and stirred for 90 minutes. Precipitation of white precipitate was observed just after the commencement of the reaction. After confirming disappearance of Boc-aminopropanol-fenbufen by TLC, diethyl ether was added to the reaction solution, and the resulting white precipitate was centrifuged. The precipitate was washed three times with diethyl ether and then dried under reduced pressure to give the titled compound (621.4 mg, yield 98%). The structure was identified by 1H-NMR (CDCl3:CD3OD=1:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07879817B2 |
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| Source dataset | uspto-grants-2011_02 |
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| ORD ID | ord-f09339abd3534153b51f036dc0ab3aa8 |
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| Source note | uspto-grants-2011_02 |
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