Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | 2-Amino-4,6-dichloropyrimidine | HCID 65522 | — |
| Reactant | HCID 66992863 | HCID 66992863 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 86626628 | HCID 86626628 | — |
Reaction Steps
A mixture of 2.563 g (11.5 mMol) 6-hydroxy-benzo[b]thiophene-3-carboxylic acid ethyl ester, 3.06 g (18.5 mMol) 2-amino-4,6-dichloropyrimidine and 5.15 g (23 mMol) K3PO4 in 87 ml NMP is stirred for 1.5 h at 60° C. Then the mixture is poured into EtOAc and water, the aq. layer separated off and extracted 3 times with EtOAc. The organic phases are washed with water and brine, dried (Na2SO4) and concentrated. Trituration in ether and filtration gives the title compound: m.p.: 178-179° C.; TLC(hexane/EtOAc 2:1): Rf=0.27. More product can be obtained from the filtrate by column chromatography (SiO2; hexane/EtOAc 3:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08058276B2 |
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| Source dataset | uspto-grants-2011_11 |
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| ORD ID | ord-a5ad343716504a35a6da85593847ea1c |
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| Source note | uspto-grants-2011_11 |
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