Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,4-Dibromobutane | HCID 8056 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 15521770 | HCID 15521770 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Hexamethylphosphoramide | HCID 12679 | — |
| Product | HCID 15521771 | HCID 15521771 | — |
Reaction Steps
0.4 g of sodium bicarbonate powder and 0.14 ml of 1,4-dibromobutane are added to 0.5 g of the compound of Example 48 in 50 ml of hexamethyl-phosphoramide. The reaction mixture is heated at 115° C. for 10 hours. The reaction mixture is hydrolysed at room temperature and extracted with ethyl acetate. The organic phase is washed several times with water and dried over anhydrous sodium sulphate and then the solvents are evaporated under reduced pressure. The residue obtained is purified by chromatography on a column of silica gel, elution being carried out with a 95/5 (v/v) cyclohexane/ethyl acetate mixture. The oil obtained is treated with hydrochloric acid in diethyl ether; M.p.=198° C. (HCl.0.4H2O).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06673790B1 |
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| Source dataset | uspto-grants-2004_01 |
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| ORD ID | ord-18b64a97df20492bad5c0b5679be6022 |
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| Source note | uspto-grants-2004_01 |
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