Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Benzenamine, 4-(3-methylphenoxy)- | HCID 151352 | — |
| Reactant | HCID 68322480 | HCID 68322480 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 53241495 | HCID 53241495 | — |
Reaction Steps
To 4-[(3-methylphenyl)oxy]aniline (90 mg, 0.45 mmol) in dichloromethane (1 mL) was added with shaking at 35° C. an aliquot of approximately ⅓ of solution 1 slowly via syringe (over ca. 1 min). After 30 min, HCl (ca. 0.8 mL) was added and the heterogeneous mixture was heated at 100° C. for 2 hours with shaking, allowing the dichloromethane to distill off through a glass capillary. After cooling to room temperature the aqueous HCl was pipetted off and the residue dried under vacuum. The residue was purified by silica gel chromatography (Biotage instrument, 10 g column) eluting with 0-100% EtOAc/cHex to give after drying the title compound as a solid (30 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09216967B2 |
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| Source dataset | uspto-grants-2015_12 |
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| ORD ID | ord-942f6cf5e9e6499da6606b24f1b4f76c |
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| Source note | uspto-grants-2015_12 |
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