Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Calcium Chloride | HCID 5284359 | — |
| Reactant | HCID 66913179 | HCID 66913179 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 66913083 | HCID 66913083 | 75% |
Reaction Steps
The synthesis method shall be explained concretely, and in order, below. A mixed solution of 2-[2-(4-methoxyphenyl)vinyl]-4,6-dimorpholino-5-nitropyrimidine (1.35 g, 3.16 mmol), zinc dust (6.19 g, 94.8 mmol), and calcium chloride (224 mg, 2.02 mmol) in acetonitrile (80 ml) and water (20 ml) was refluxed under heating for 1 hour. The undissolved matter was separated out by celite filtering, the filtrate was distilled away under reduced pressure, water was added to the residue, the precipitated crystals were taken out by filtering, and 5-amino-2-[2-(4-methoxyphenyl)vinyl]-4,6-dimorpholinopyrimidine (940 mg, yield 75%) was obtained. The melting point measurement result, the MS measurement result, and the NMR data for the obtained Compound 131 are shown below.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08563715B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-6931fadb52a141559e920e5511468f5d |
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| Source note | uspto-grants-2013_10 |
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