Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | 4-Hydroxy-3-methoxy-5-nitrobenzoic acid | HCID 15527939 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 89619537 | HCID 89619537 | — |
Reaction Steps
A suspension of compound of Example 1a (1.0 eq) in DCM (approx 3.4 vol) is treated with thionyl chloride (1.0-1.2 eq, for example 1.1 eq) and catalytic amount (0.011 eq) of DMF and the mixture is stirred for 16 h at 40° C. DCM is distilled off (approx 2.7 vol) and the residue is diluted with THF (approx 1.8 vol). The excess of thionylchloride is distilled off with THF/DCM and the residue after distillation is cooled to 10° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09126988B2 |
|---|
| Source dataset | uspto-grants-2015_09 |
|---|
| ORD ID | ord-e965651e96d24725bfd69053be7f9cf5 |
|---|
| Source note | uspto-grants-2015_09 |
|---|
