HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexamethylenetetramine → 3,5-Difluoro-4-hydroxybenzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexamethylenetetramine | HCID 4101 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 2,6-Difluorophenol | HCID 94392 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3,5-Difluoro-4-hydroxybenzaldehyde | HCID 10192584 | — |
Reaction Steps
TFA (7 mL) was added to 2,6-difluoro-phenol (1.0 g, 7.69 mmol) and hexam-ethylenetetraamine (1.08 g, 7.69 mmol), and the mixture was stirred at 75˜80° C. for 12 hours. The reactant was cooled, diluted with water, and then extracted with DCM/MeOH (9:1) solution three or four times. The organic layer was concentrated under reduced pressure, and DCM was added to the residue. The mixture was dried with MgSO4 and concentrated under reduced pressure. The reaction product was used in the next step without a separate purification process.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447044B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-027e21b1ee4d42b3bf74111e4af661b8 |
| Source note | uspto-grants-2016_09 |