Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 2-Amino-4,6-dichloropyrimidine | HCID 65522 | — |
| Reactant | HCID 17797766 | HCID 17797766 | — |
| Product | HCID 385279 | HCID 385279 | 50.8% |
Reaction Steps
60% Sodium hydride (0.4 g, 0.01 mol) was suspended in dry dioxane (40 ml) and dihydroxymethylcyclobutane (1.16 g, 0.01 mol) dissolved in dry dioxane (40 ml) was dropwise added thereto. The mixture was stirred at 60-70° C. for 30 minutes, and 2-amino-4,6-dichloropyrimidine (1.64 g, 0.01 mol) was added. The mixture was refluxed for 3 hours, and filtrated. The solvent in the filtrate was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=50:1) to give white crystals (1.24 g, 50.8%), m.p. 125-127° C. (acetone).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06080750 |
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| Source dataset | uspto-grants-2000_06 |
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| ORD ID | ord-febe5ae2d7c14114a4b2a1d8060a7cc7 |
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| Source note | uspto-grants-2000_06 |
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