Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 86691932 | HCID 86691932 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Product | HCID 86691933 | HCID 86691933 | — |
Reaction Steps
7-Methyl-4-nitroso-2-phenyl-3,4-dihydro-2H-benzo[b][1,4]oxazine (1.5 g) was dissolved in acetone (90 mL). To it was added saturated NH4Cl solution (4.6 mL) followed by water (4.6 mL) with constant stirring until a homogenous solution resulted. The reaction mixture was cooled to 0° C., and to it was added zinc dust (1.5 g) in small portions. After addition, the mixture was stirred at RT for 2 h. Reaction was monitored by TLC. After completion of reaction, the mixture was concentrated under reduced pressure, and water (100 mL) was added. The mixture was extracted with DCM (3×100 mL). The organic layer was dried over sodium sulfate and concentrated under reduced pressure. The crude product was dried under high vacuum (1.5 g), which was carried forward to the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09193728B2 |
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| Source dataset | uspto-grants-2015_11 |
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| ORD ID | ord-a21fec5b28ef4ee5800f839813a801d3 |
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| Source note | uspto-grants-2015_11 |
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