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35
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64549163869
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note
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2 (3 × 5 mL). The combined organic layer was dried over 4 Å molecular sieves and the solvent was removed under reduced pressure. The crude amine was employed immediately in the oxidation reaction.
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45
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0000835314
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de Meijere A. (Ed), Thieme, Stuttgart
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47
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0000818721
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For the preparation of DMDO solution, see:
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For the preparation of DMDO solution, see:. Crandall J.K., Batal D.J., Sebesta D.P., and Lin F. J. Org. Chem. 56 (1991) 1153
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48
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64549132319
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note
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General procedure for the oxidation of amines 1b-f with DMDO. Free amine 1 (0.5 mmol) in acetone (1 mL) was added to a 0.08 M solution of DMDO in acetone (45 mL). The resulting mixture was maintained at room temperature for 1 h in the dark. The solvent was removed on a rotary evaporator under normal pressure. The crude product was purified by column chromatography (eluent: chloroform). The resulting nitrocyclopropanes 8a,c,d,f are stable on storage at 5 °C over a long time.
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-
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49
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64549156291
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note
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+: 159.12, found: 159.10.
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