1-氯乙基 辛基 碳酸盐

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 10.6 g (0.045 mole) of previously distilled octyl 1-chloroethyl carbonate, 4.5 g (0.08 mole) of dry KF and 0.6 g (0.002 mole) of 18-crown-6 ether is stirred and warmed at about 85° C. (oil bath ) under a pressure of about 1.87 kPa. After 12 hrs., all the volatile acetaldehyde has evaporated. The mixture is cooled and distilled under reduced pressure. There is obtained 6.87 g of pure n-octyl fluoroformate (86%). b.p.: 74°-77° C. at 533 Pa (4 mmHg). , all the volatile acetaldehyde has evaporated The mixture is cooled distilled under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 10.6 g (0.045 mole) of previously distilled octyl 1-chloroethyl carbonate, 4.5 g (0.08 mole) of dry KF and 0.6 g (0.002 mole) of 18-crown-6 ether is stirred and warmed at about 85° C. (oil bath ) under a pressure of about 1.87 kPa. After 12 hrs., all the volatile acetaldehyde has evaporated. The mixture is cooled and distilled under reduced pressure. There is obtained 6.87 g of pure n-octyl fluoroformate (86%). b.p.: 74°-77° C. at 533 Pa (4 mmHg). , all the volatile acetaldehyde has evaporated The mixture is cooled distilled under reduced pressure

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirring solution of dry n-octanol (6.42 g, 49.3 mmol) and pyridine (3.90 g, 49.3 mmol) in anhydrous ether (75 mL) was added at 0° C. alpha-chloroethyl chloroformate (prepared according to U.K. Pat. No. 1,426,717; 7.00 g, 49.3 mmol). The mixture was stirred vigorously for three hours at 25° C. then filtered. The filtrate was concentrated in vacuo and distilled at 102°-107° C. (2 mm) affording 8.1 g title product as a clear oil (34.2 mmol, 69.4%): 1H NMR (CDCl3) delta 0.44-2.03 (m, 15H), 1.60 (d, J=6 Hz, 3H), 3.94 (t, J=7 Hz, 2H), 6.18 (q, J=6 Hz, 1H). prepared then filtered The filtrate was concentrated in vacuo distilled at 102°-107° C. (2 mm)

反应条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 10.6 g (0.045 mole) of previously distilled octyl 1-chloroethyl carbonate, 4.5 g (0.08 mole) of dry KF and 0.6 g (0.002 mole) of 18-crown-6 ether is stirred and warmed at about 85° C. (oil bath ) under a pressure of about 1.87 kPa. After 12 hrs., all the volatile acetaldehyde has evaporated. The mixture is cooled and distilled under reduced pressure. There is obtained 6.87 g of pure n-octyl fluoroformate (86%). b.p.: 74°-77° C. at 533 Pa (4 mmHg). , all the volatile acetaldehyde has evaporated The mixture is cooled distilled under reduced pressure