Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitrofungin | HCID 12074 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 86639105 | HCID 86639105 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67523903 | HCID 67523903 | 67.6% |
Reaction Steps
370 mg (14.7 mmol) sodium hydride was given to a solution of 2.31 g (13.3 mmol) 2-chloro-4-nitrophenol in 25 ml DMF. Stirring was continued for 30 min. at room temperature. 2.50 g (13.3 mmol) 3-(4-Chloro-pyrimidin-2-ylamino)-propan-1-ol were added and the mixture heated to 140° C. for 24 h. The reaction mixture was evaporated, taken up with water and extracted with dichloromethane. The organic phase was extracted with sodium carbonate solution, dried (sodium sulphate) and evaporated. The obtained material was dissolved in 3 ml dichloromethane and purified by chromatography over silica (dichloromethane/ethanol 95:5) to give 2.92 g (67%) 3-[4-(2-chloro-4-nitro-phenoxy)-pyrimidin-2-ylamino]-propan-1-ol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08080552B2 |
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| Source dataset | uspto-grants-2011_12 |
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| ORD ID | ord-747279c928104cbbaffe30bd51801587 |
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| Source note | uspto-grants-2011_12 |
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