Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nanofin | HCID 68843 | — |
| Reactant | 1-(Diphenylmethyl)azetidin-3-yl methanesulfonate | HCID 2758716 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 21836512 | HCID 21836512 | 0.1% |
Reaction Steps
1-Diphenylmethyl-3-methanesulphonyloxyazetidine (see Preparation 54) (2 g, 1 mol. equiv.) and 2,6-dimethylpiperidine (6.79 ml, 3 mol. equiv.) were heated together at 110° C. under nitrogen for six hours. Saturated aqueous sodium bicarbonate solution (60 ml) was added and the mixture extracted with ethyl acetate (3×40 ml). The combined organic extracts were dried using magnesium sulphate. The organic solvent was removed under reduced pressure and the residue purified by flash column chromatography on silica gel eluting with methanol:dichloromethane (1:9, by volume) to give the title compound (0.48 g). TLC Rf=0.39 (silica, methanol:dichloromethane, 1:9, by volume). LRMS m/z=335 (m+1)+. Found: C, 80.29; H, 9.00; N, 8.14. C23H30N2 0.125 CH2Cl2 requires C, 80.48; H, 8.84; N, 8.12%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05968923 |
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| Source dataset | uspto-grants-1999_10 |
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| ORD ID | ord-57f0379365174b8caa3ace0576416c12 |
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| Source note | uspto-grants-1999_10 |
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