Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Phthalimide | HCID 6809 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 15237992 | HCID 15237992 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 54369707 | HCID 54369707 | 61.1% |
Reaction Steps
To a solution of methyl (2-hydroxymethyl-l,2,3,4-tetrahydronaphthalen-5-yl)oxyacetate (1.15 g), phthalimide (1.22 g) and triphenylphosphine (2.17 g) in tetrahydrofuran (50 ml) was added diethyl azodicarboxylate (1.6 ml) at -20° C. After stirred for 2 h, the mixture was quenched by addition of water. The mixture was extracted with ether. The extract was washed with a saturated aquous solution of sodium chloride, dried over anhydrous magnesium sulfate and evaporated. To a solution of the obtained residue in ethanol (30 ml) was added hydrazine monohydrate (0.7 ml) at room temperature. The mixture was stirred overnight. The mixture was quenched by addition of water (20 ml) and evaporated. The residue was crystallized from 2N hydrochloric acid (20 ml) to give the title compound (700 mg) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05596009 |
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| Source dataset | uspto-grants-1997_01 |
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| ORD ID | ord-cbaff100a4d04d27ae0f5adff75149ad |
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| Source note | uspto-grants-1997_01 |
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