HuagongsheHuagongshe Chemistry Print Report · For research reference only
4,6-Dichloropyrimidine → HCID 86711520, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4,6-Dichloropyrimidine | HCID 70943 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | 4-Amino-1-naphthol hydrochloride | HCID 2723858 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86711520 | HCID 86711520 | — |
Reaction Steps
To a solution of 4-aminonaphthalen-1-ol hydrochloride (6.82 g, 31.4 mmol) in acetonitrile (80 mL) at 0° C. was added drop-wise DBU (11.0 mL, 75.0 mmol). After 10 min 4,6-dichloropyrimidine (5.00 g, 34.0 mmol) was added portion-wise over 5 min and the reaction mixture warmed to RT for 3 hr and then evaporated in vacuo. The residue was diluted with water (250 mL) and sonicated for 15 min and then stirred at RT for 16 hr. The resulting precipitate was isolated by filtration, washed with water (3×100 mL) and dried in vacuo to afford the title compound, Intermediate E3, as a grey solid (8.27 g, 97%); Rt 1.85 min (Method 2, acidic); m/z 272 (M+H)+, (ES+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09249125B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-78f48944e29d433eaed5e7e6190af2fc |
| Source note | uspto-grants-2016_02 |