HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → 3-(3-Chloropropoxy)-4-methoxy-6-nitrobenzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 3-(3-Chloropropoxy)-4-methoxy-6-nitrobenzaldehyde | HCID 25051844 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 3-(3-Chloropropoxy)-4-methoxy-6-nitrobenzoic acid | HCID 23033004 | 86% |
Reaction Steps
Methanol (4 lt), 3-(3-chloropropoxy)-4-methoxy-6-nitro benzaldehyde (560 gm) and 30% methanolic NaOH solution (5 ml) were heated to 45° C. To this reaction mass 35% of H2O2 solution (1200 ml) was added drop wise in 3-4 hours maintaining a pH of 10.5-11.5 with 30% methanolic NaOH solution. The reaction mass was quenched into ice water (10 kg) and the pH adjusted to 2.0-3.0 using hydrochloric acid. The solid obtained was filtered, washed with 50% aqueous methanol (500 ml) and dried at 45-50° C. to yield the title compound (510 gm, 86% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08350029B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-9e41eda3d26c4256933a81a477637ade |
| Source note | uspto-grants-2013_01 |