Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | 4-Bromoaniline | HCID 7807 | — |
| Reactant | Sodium Cyanide | HCID 8929 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | Nitrosylsulfuric acid | HCID 82157 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Reactant | HCID 178418260 | HCID 178418260 | — |
| Reactant | HCID 178418546 | HCID 178418546 | — |
| Product | Benzoic Acid | HCID 243 | — |
Reaction Steps
Scheme 1 illustrates a representative synthesis of a 6-substituted 4-bromo-2-bromomethyl-benzoic acid methyl ester from commercially available precursors wherein the respective reaction steps comprise as follows: (a) NaNO2, aq. HCl; (b) NaCN, CuCN and HCl; (c) NaOH; (d) nitrososulphuric acid; (e) MeI and K2CO3, and (f) NBS and (PhCO2)2. Briefly, a 4-bromo-aniline may be diazotized under Sandmeyer reaction conditions, followed by conversion to the nitrile using sodium cyanide and copper cyanide. The nitrile may then be hydrolyzed to an amide by basic hydrolysis. The amide can then be hydrolyzed with nitrososulphuric acid to provide a benzoic acid, which may be converted to a methyl ester under standard conditions. The benzylic methyl group may be monobrominated with N-bromosuccinimide using benzoyl peroxide as a radical initiator to yield a desired 6-substituted 4-bromo-2-bromomethyl-benzoic acid methyl ester.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07888353B2 |
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| Source dataset | uspto-grants-2011_02 |
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| ORD ID | ord-b13ddf84d7ca436ba9d38ca11b9eab7e |
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| Source note | uspto-grants-2011_02 |
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