Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Amino-4,6-dichloropyrimidine | HCID 65522 | — |
| Reactant | HCID 86618286 | HCID 86618286 | — |
| Solvent | Acetone | HCID 180 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59596367 | HCID 59596367 | — |
Reaction Steps
A mixture of 567 mg (1.62 mMol) of 7-hydroxy-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid (3-trifluoromethyl-phenyl)-amide (Step 6.2), 532 mg (3.24 mMol) 2-amino-4,6-dichloro-pyrimidine and 145 mg (3.62 mMol) NaOH in 5 ml acetone, 7 ml H2O and 3 ml DMF is stirred at 60° C. for 24 h. Then it is poured into 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. Column chromatography (SiO2; hexane/EtOAc 2:1→3:2) gives the title compound: m.p.: 175° C.; MS: [M+1]+=478/480; Anal.: C,H,N,Cl.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07855215B2 |
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| Source dataset | uspto-grants-2010_12 |
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| ORD ID | ord-4f08f0e704d144c2ab06f7ebdb90fbc2 |
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| Source note | uspto-grants-2010_12 |
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