Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Homoveratrylamine | HCID 8421 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | (3-Bromophenyl)acetic acid | HCID 74653 | — |
| Solvent | Benzene | HCID 241 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58906470 | HCID 58906470 | — |
Reaction Steps
2-(3-Bromo-phenyl)-N-[2-(3,4-dimethoxy-phenyl)-ethyl]-acetamide (41) was prepared as follows: A solution of 3-bromo-phenylacetic acid (2.0 g, 9.3 mmol) and oxalyl chloride (36.4 g, 0.287 mol) in 80 mL of benzene was refluxed for 6 h. The solution was evaporated with benzene 3 times and dried in vacuum. A solution of 3-bromo-phenylacetic acid (1.1 eq.) in CH2Cl2 was added to mixture of 100 mL of 1N NaOH and solution of 3,4-di-methoxy-phenethylamine (1.31 g, 7.22 mmol) in 100 mL of CH2Cl2. The reaction mixture was stirred overnight at r.t. Another portion of acid chloride (0.1 eq.) in 10 mL of CH2Cl2 was added and stirred for 1 h. Organic phase was separated, washed with 1N HCl, 1N NaOH, water, dried over Na2SO4, filtered and evaporated. A residue was crystallized from EtOAc-hexanes mixtures. Yield is 2.59 g (95%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07718672B2 |
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| Source dataset | uspto-grants-2010_05 |
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| ORD ID | ord-53d9ccdb9d1444ad89aa47688db8703d |
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| Source note | uspto-grants-2010_05 |
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