Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | 2,6-Dichlorobenzaldehyde | HCID 6737 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Hydroxylamine sulfate | HCID 24846 | — |
| Product | HCID 23295251 | HCID 23295251 | — |
Reaction Steps
Starting from 2,6-dichlorobenzaldehyde 75 g (0.43 mol) of 2,6-dichlorobenzaldehyde were dissolved in 400 ml of toluene and then 155 g (0.24 mol) of 25% strength hydroxylammonium sulfate solution were added. At 75° C., 38 g of 50% strength NaOH were added dropwise. After stirring for half an hour, the phases were separated at 75° C., and the organic phase was washed with water and then cooled. At 25° C., 276 g (0.46 mol) of 12.5% strength sodium hypochlorite solution were added dropwise over 4-6 h while simultaneously passing in ethylene. After addition of the hypochlorite solution was complete, the mixture was stirred for 1 h, the phases were separated, the organic phase was washed with water, and the solvent was distilled off under reduced pressure. 82 g (89% of theory) of the required product were obtained with a purity (by GC) of 96%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06124469 |
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| Source dataset | uspto-grants-2000_09 |
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| ORD ID | ord-4acb424308c440e781d5dcd2ebf8d50e |
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| Source note | uspto-grants-2000_09 |
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