HuagongsheHuagongshe Chemistry Print Report · For research reference only
4,6-Dichloropyrimidine → HCID 11503607, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4,6-Dichloropyrimidine | HCID 70943 | — |
| Reactant | HCID 86618286 | HCID 86618286 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 11503607 | HCID 11503607 | — |
Reaction Steps
A mixture of 1.00 g (2.85 mMol) of 7-hydroxy-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid (3-trifluoromethyl-phenyl)-amide (Step 6.2) and 447 mg (3.0 mMol) 4,6-dichloro-pyrimidine in 8 ml acetone, 5 ml H2O and 3 ml NaOH 1 M is stirred at rt for 5 h. The reaction mixture is diluted with water and EtOAc, the aqueous phase separated off and extracted twice with EtOAc. The organic layers are washed with water and brine, dried (Na2SO4) and concentrated. Chromatography (Combi Flash; hexane/EtOAc 19:1→7:3→1:4) gives the title compound: m.p.: 120° C.; MS: [M+1]+=463/465; Anal.: C,H,N,F,Cl.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07855215B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-9d68bf64dfb143dd99a1c5e93a179394 |
| Source note | uspto-grants-2010_12 |