HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetaldehyde → HCID 90412925, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetaldehyde | HCID 33 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 6-Amino-3-methylpicolinic acid | HCID 90412282 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 90412925 | HCID 90412925 | 72.8% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
To the title compound of Step A (340 mg, 2.2 mmol) in H2O (7 mL) was added 1M aq. NaOH (2.2 mL, 2.2 mmol) and chloroacetaldehyde (210 μL, 3.4 mmol) and the reaction mixture heated in a microwave reactor at 150° C. for 2 h. Additional 1M aq. NaOH (2.2 mL, 2.2 mmol) and chloroacetaldehyde (210 μL, 3.4 mmol) were added and heating continued at 150° C. for 2 h. The reaction was purified via prep HPLC to give the title compound (282 mg, 72%). MS (ESI) mass calcd. for C9H8N2O2, 176.1; m/z found 177.0 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09062078B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-70218fa18f3e41579a0c2898fc8eb921 |
| Source note | uspto-grants-2015_06 |