反应详情

N-(2-(1H-Indene-1-yl)ethyl)hydroxylamine (85 mg, 0.486 mmol) was added to a slurry of zinc dust (104 mg, 1.59 mmol) in glacial acetic acid (3 ml), and the mixture was heated at 65° for 2 hours. The mixture was cooled and filtered, then made basic with conc. ammonium hydroxide and extracted with ether. The ether layer was washed with water, then with brine, dried ober sodium sulfate, filtered, and evaporated to dryness in vacuo. The residue was chromatographed on a silica gel column eluted with 90:10:1 of CH2Cl2 :MeOH:NH4OH. The product fractions were evaporated to dryness in vacuo to give (2-(1H-indene-3-yl)ethyl)amine.

1. temperaturethe mixture was heated at 65° for 2 hours
2. temperatureThe mixture was cooled
3. filtrationfiltered
4. extractionextracted with ether
5. washThe ether layer was washed with water
6. dry with materialwith brine, dried ober sodium sulfate
7. filtrationfiltered
8. customevaporated to dryness in vacuo
9. customThe residue was chromatographed on a silica gel column
10. washeluted with 90:10:1 of CH2Cl2
11. customThe product fractions were evaporated to dryness in vacuo