Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 13062442 | HCID 13062442 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 13062448 | HCID 13062448 | 94.5% |
Reaction Steps
A mixture of trans-3,4-dichloro-N-methyl-N-[7-(1-pyrrolidinyl)-1,4-dioxaspiro[4.5]dec-8-yl]benzeneacetamide (12.3 g, 0.029 mol) from Example 1, 3 N HCl solution (288 ml), and 432 ml of acetone was stirred at 60° C. under N2 atmosphere for one hour. Acetone was removed on a rotary evaporator and the mixture was extracted with chloroform. The chloro-form extracts were dried (Na2SO4), concentrated in vacuo and diluted with ether. Refrigeration overnight gave white crystals which were dried at 60° C. in vacuo for two days to give 10.5 g (87%) of the titled compound, mp 148.0°-148.9° C. The mass spectrum indicated ion fragments at m/e 382/384 (M+, chlorine isotopic peaks). The ir and nmr spectra were consistent with the structure assignment.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04360531 |
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| Source dataset | uspto-grants-1982_11 |
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| ORD ID | ord-5363d821799249ac8111317fa0956901 |
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| Source note | uspto-grants-1982_11 |
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