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Reaction id: 0501011029_01, verified by Personal Chemistry ©
4
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Phosphorus ...
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dry 1,4-dioxane
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5p
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Yield: 82% Time: 1500s Temperature: 120 °C
Chemicals
| Name |
MW [g/mol] |
Density [g/ml] |
Amount [mmol] |
Mass/Volume |
| Substrate 1 |
175.187 |
1.000 |
1.712 |
300.000 mg |
| Phosphorus oxychloride |
153.332 |
1.645 |
3.433 |
320.000 µl |
| dry 1,4-dioxane |
88.106 |
1.034 |
23.472 |
2000.000 µl |
| Product 1 |
193.633 |
1.000 |
0.000 |
0.000 mg |
Keywords
Chlorination, Halogenation, Substitution
Comments
Synthesis: This reaction requires 3 h at 106°C with POCl3 as solvent to go to completion using conventional heating.
Before microwave heating, the reaction mixture was stirred for 2 min at room temperature to make it homogeneous. The reaction was also scaled up to 16 mmol and then gave 80% yield.
Work-up and purification: After the reaction, the mixture was poured into ice-water (20 ml). The resulting solution was then neutralised using 0.5 M KOH and stirred for 20 min. The precipitate was then filtered off and washed with water to give the pure product.
Characterisation: By MS and 1H NMR.
Instrument Settings
Absorption level: Normal
Pre-stirring time: 0s
References
Glasnov, T. N.; Stadlbauer, W.; Kappe, C. O. J Org Chem 2005, 70, 3864-3870
Analysis
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