反应详情

温度

-70 °C

(±) 3-(N-Methyl-N-methoxyaminocarbonyl)-1-azabicyclo[2.2.2]octane (D31) (6.0g, 0.03 moles) was dissolved in dry toluene (250ml) and cooled to -70° C. under a nitrogen atmosphere. Diisobutylaluminium hydride (1.5M solution in toluene (45ml, 0.068 moles) was added dropwise. The reaction was then allowed to warm to room temperature over a period of 2h. Hydrochloric acid (2N, 300ml) was added rapidly with vigorous stirring. The aqueous layer was saturated with potassium carbonate and the mixture extracted with chloroform (3×250ml). The combined extracts were dried (Na2SO4) and evaporated to dryness. The residue was distilled in a Kugelrohr to yield the title compound (D32) as a colourless oil (3.6g, 85%) b.p. 100° C. at 1.0

1. temperatureto warm to room temperature over a period of 2h
2. extractionthe mixture extracted with chloroform (3×250ml)
3. dry with materialThe combined extracts were dried (Na2SO4)
4. customevaporated to dryness
5. distillationThe residue was distilled in a Kugelrohr