2-(bromomethyl)oxolane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 24.9 gm (0.1 mol) of 2-(p-methoxybenzyl)-3,4-dimethyl-4-hydroxy-piperidine were stirred in 200 ml of dimethylformamide in the presence of 12.6 gm of sodium bicarbonate for 24 hours at 100° C with 19.7 gm (0.12 mol) of tetrahydrofurfuryl bromide. Subsequently, the reaction mixture was evaporated in vacuo, and the residue shaken with a mixture of 150 ml of chloroform and 100 ml of water. After isolation in a separating funnel, the aqueous phase was extracted once more with 50 ml of chloroform. The combined chloroform extracts were washed with water, dried with sodium sulfate and evaporated in vacuo. In analogy to the procedure described in Example 1, the residue was purified by column-chromatography on aluminum oxide (700 gm, activity stage III, neutral), using chloroform as the flow agent. After evaporation of the combined eluates comprising the pure product, a residue of 16 gm was obtained, which was further reacted as such in the following step. Subsequently, the reaction mixture was evaporated in vacuo After isolation in a separating funnel, the aqueous phase was extracted once more with 50 ml of chloroform The combined chloroform extracts were washed with water dried with sodium sulfate evaporated in vacuo the residue was purified by column-chromatography on aluminum oxide (700 gm, activity stage III, neutral) After evaporation of the combined eluates a residue of 16 gm was obtained which was further reacted as such in the following step

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 165 g of tetrahydrofurfuryl bromide, 348 g of morpholine, 5 g of sodium iodide and 500 g of tetrahydrofuran was heated under reflux for 50 hours. After cooling, diethyl ether was added to the reaction solution, which was filtered, concentrated in vacuum and purified by vacuum distillation, whereby 158 g of 4-tetrahydrofurfuryl-morpholine, designated [B-44], was obtained (boiling point 64° C./15 Pa, yield: 92%). was heated under reflux for 50 hours After cooling was filtered concentrated in vacuum purified by vacuum distillation, whereby 158 g of 4-tetrahydrofurfuryl-morpholine was obtained (boiling point 64° C./15 Pa, yield: 92%)