Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | Phthalohydrazide | HCID 11367556 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 71129228 | HCID 71129228 | 75% |
Reaction Steps
The general procedure from H. J. Barber et. al. Journal of the Chemical Society, 1948, page 1458 was followed. A 250 mL round bottom flask equipped with a magnetic stir bar and a condenser further attached to a N2 source was charged with 10.0 g (61.7 mmol, available from Aldrich,) phthalhydrazide, 9.57 g (191 mmol, available from Aldrich) hydrazine hydrate, and 60 mL of water. The mixture was heated to 90° C. at which point it became substantially homogeneous, then filtered while warm. The filtrate was added to about 1 L of ethanol then the precipitate was collected by filtration and dried in vacuo at room temperature to afford 9.0 g (46 mmol, 75% yield) of fluffy, white powder. TGA analysis showed 15.7 wt % loss by 150° C. (16.5% is theoretical loss of hydrazine).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08338542B1 |
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| Source dataset | uspto-grants-2012_12 |
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| ORD ID | ord-bce113488458423daef15170d5bb26f0 |
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| Source note | uspto-grants-2012_12 |
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