反应详情

(3-Nitro)phenyl methyl sulphone (prepared as described in Step 1 above) (5.396 g) reduced iron (7.5 g) and ammonium chloride (7.18 g) were mixed together in ethanol/water (2:1) (150 ml) and heated under reflux for 2 hours. The black solution was filtered through `Celite` and the pad washed with ethyl acetate. The solvents were removed under reduced pressure and the residue taken up in ethyl acetate/water. The organic layer was separated and the aqueous layer extracted with 3 further portions of ethyl acetate. The combined organic layers were washed with brine and the solvent removed under reduced pressure to give a dark orange oil (3.9275 g). This was chromatographed on silica gel using ethyl acetate-hexane (45:55 to 50:50) as eluant to give the title compound as an orange oil, yield 3.607 g.

1. temperatureheated
2. temperatureunder reflux for 2 hours
3. filtrationThe black solution was filtered through `Celite` and the pad
4. washwashed with ethyl acetate
5. customThe solvents were removed under reduced pressure
6. customThe organic layer was separated
7. extractionthe aqueous layer extracted with 3 further portions of ethyl acetate
8. washThe combined organic layers were washed with brine
9. customthe solvent removed under reduced pressure