HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetyl chloride → HCID 9801028, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetyl chloride | HCID 6577 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Phthalazine, 4-[(3,5-dichloro-4-pyridinyl)methyl]-1,2-dihydro-7-methoxy- | HCID 9797215 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9801028 | HCID 9801028 | 110.5% |
Reaction Steps
At room temperature, under N2 and stirring, a solution of 1-[4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-1H-phthalazine (1.9 g, 5.9 mmoles), prepared as described in example 22, in dry THF (70 ml) was added with triethylamine (2.05 ml, 14.7 mmoles) and cooled at 0° C. Chloroacetyl chloride (0.56 ml, 7.07 mmoles) was dropwise added and a precipitate formed. After 1 night further 50% of triethylamine and chloroacetyl chloride was added, and after 20 hours at room temperature the mixture was poured into water/ice, concentrated and extracted more times with CH2Cl2. The organic phase was washed with water, anhydrified and brought to dryness to give 2.6 g of the title compound (quantitative yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06492360B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-29642a82033c4f32bf78d039ada9df73 |
| Source note | uspto-grants-2002_12 |