Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Hexamethylenetetramine | HCID 4101 | — |
| Reactant | 4-(Bromomethyl)phenylacetic acid | HCID 4519056 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 2-(4-formylphenyl)acetic Acid | HCID 11344187 | — |
Reaction Steps
The title compound was synthesized by referring to Org. Synth., 1963, IV, 690. A suspension of (4-bromomethylphenyl)acetic acid (6.0 g) and hexamethylenetetramine (11.1 g) in ethanol (80 ml) was stirred for 2 hours at 100° C., then acetic acid (20 ml) and water (20 ml) were sequentially added thereto followed by stirring for 1.5 hours at 100° C. The solvent was evaporated in vacuo, extracted with ethyl acetate, then sequentially washed with water and brine, dried over anhydrous magnesium sulfate, and then the solvent was evaporated in vacuo. A solution of the residue in tetrahydrofuran was filtered through silica gel, then the solvent was evaporated in vacuo, and the resulting solid was washed with a hexane-diethyl ether system to provide the title compound (2.0 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08399520B2 |
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| Source dataset | uspto-grants-2013_03 |
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| ORD ID | ord-aa9a57bad32e4ef8a4c93b5b1c5ffa7b |
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| Source note | uspto-grants-2013_03 |
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