ETHYL 2-(TETRAHYDRO-2H-PYRAN-2-YLOXY)CYCLOPROPANECARBOXYLAT

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In an autoclave, a solution of 0.25 mol of the compound obtained in Step 2, 2 g of sodium cyanide, 300 ml of a 2N solution of ammonia in methanol and 80 ml of liquid ammonia is heated at 65° C. for 5 days and is then concentrated to dryness. The residue is taken up in a mixture of dichloromethane/saturated potassium carbonate solution, filtered over Celite and then treated in conventional manner. After evaporating under reduced pressure, the residue is triturated in petroleum ether, filtered, rinsed and dried, allowing the expected product to be isolated. is then concentrated to dryness The residue is taken up in a mixture of dichloromethane/saturated potassium carbonate solution filtered over Celite treated in conventional manner After evaporating under reduced pressure the residue is triturated in petroleum ether filtered rinsed dried to be isolated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In an autoclave, a solution of 0.25 mol of the compound obtained in Step 2, 2 g of sodium cyanide, 300 ml of a 2N solution of ammonia in methanol and 80 ml of liquid ammonia is heated at 65° C. for 5 days and is then concentrated to dryness. The residue is taken up in a mixture of dichloromethane/saturated potassium carbonate solution, filtered over Celite and then treated in conventional manner. After evaporating under reduced pressure, the residue is triturated in petroleum ether, filtered, rinsed and dried, allowing the expected product to be isolated. is then concentrated to dryness The residue is taken up in a mixture of dichloromethane/saturated potassium carbonate solution filtered over Celite treated in conventional manner After evaporating under reduced pressure the residue is triturated in petroleum ether filtered rinsed dried to be isolated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 0.75 mol of the compound obtained in Step 1 in 200 ml of ether there are added 1.5 g of rhodium acetate and then, over 6 hours, a solution of 93 g of ethyl diazoacetate in 50 ml of ether. After stirring at ambient temperature for 16 hours, the reaction mixture is filtered and is then distilled at 50-90° C. and 0.5 torr. The residue obtained is redistilled at 80-84° C. and 0.2 torr, allowing the expected product to be isolated. the reaction mixture is filtered is then distilled at 50-90° C. The residue obtained is redistilled at 80-84° C. to be isolated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In an autoclave, a solution of 0.25 mol of the compound obtained in Step 2, 2 g of sodium cyanide, 300 ml of a 2N solution of ammonia in methanol and 80 ml of liquid ammonia is heated at 65° C. for 5 days and is then concentrated to dryness. The residue is taken up in a mixture of dichloromethane/saturated potassium carbonate solution, filtered over Celite and then treated in conventional manner. After evaporating under reduced pressure, the residue is triturated in petroleum ether, filtered, rinsed and dried, allowing the expected product to be isolated. is then concentrated to dryness The residue is taken up in a mixture of dichloromethane/saturated potassium carbonate solution filtered over Celite treated in conventional manner After evaporating under reduced pressure the residue is triturated in petroleum ether filtered rinsed dried to be isolated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 0.75 mol of the compound obtained in Step 1 in 200 ml of ether there are added 1.5 g of rhodium acetate and then, over 6 hours, a solution of 93 g of ethyl diazoacetate in 50 ml of ether. After stirring at ambient temperature for 16 hours, the reaction mixture is filtered and is then distilled at 50-90° C. and 0.5 torr. The residue obtained is redistilled at 80-84° C. and 0.2 torr, allowing the expected product to be isolated. the reaction mixture is filtered is then distilled at 50-90° C. The residue obtained is redistilled at 80-84° C. to be isolated