6-methoxyhexan-1-ol

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: 803.6 grams of the monomethyl ether described in Part (A) above were azeotropically esterified with 629.8 grams acrylic acid in 254.6 grams toluene in the presence of 24 grams p-toluenesulfonic acid and inhibitors until no more water was collected. Conditions were 95°-98° C., nitrogen sparge in vacuo. On completion, the product was washed and neutralized with sodium carbonate. 900 ppm p-methoxyphenol (MEHQ) was added and the solvent removed at 80° C. with maximum vacuum in the presence of an air sparge. Filter aid was added and the product filtered at 60° C. to give a clear, yellow liquid having a viscosity of 6.5 cps and a Gardener color of 3. Equipment used was a 2 liter flask, thermometer, Dean-Stark condenser and sparge tube. was collected were 95°-98° C. nitrogen sparge in vacuo On completion, the product was washed 900 ppm p-methoxyphenol (MEHQ) was added the solvent removed at 80° C. with maximum vacuum in the presence of an air sparge Filter aid was added the product filtered at 60° C. to give a clear, yellow liquid thermometer, Dean-Stark condenser and sparge tube

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

実験手順: 6-Methoxy-hexanol (8.16 g) was oxidized with Jones reagent (2.67-M, 53 ml) in acetone (100 ml) at -10 ° C. to give 6.17 g of 6-methoxy-caproic acid.

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

実験手順: Sodium hydride (NaH) (50%, 6.12 g) suspended in tetrahydrofuran (THF) (60 ml) was added to a solution of 1,6-hexanediol (15.0 g) in THF (200 ml), and kept at 60° C. until gas evolution stopped. After cooling, a solution of methyl iodide (12 ml) in THF (35 ml) was added and kept overnight at room temperature. The crude product obtaind after the usual work-up was chromatographed to give 6-methoxy-1-hexanol. Yield; 8.16 g kept at 60° C. until gas evolution After cooling The crude product obtaind after the usual work-up was chromatographed

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

実験手順: 6-Methoxy-hexanol (8.16 g) was oxidized with Jones reagent (2.67-M, 53 ml) in acetone (100 ml) at -10° C. to give 6.17 g of 6-methoxy-caproic acid.

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

実験手順: 6-Methoxy-hexanol (8.16 g) was oxidized with Jones reagent (2.67-M, 53 ml) in acetone (100 ml) at -10° C. to give 6.17 g of 6-methoxy-caproic acid.

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

実験手順: Sodium hydride (NaH) (50%, 6.12 g) suspended in tetrahydrofuran (THF) (60 ml) was added to a solution of 1,6-hexanediol (15.0 g) in THF (200 ml), and kept at 60° C. until gas evolution stopped. After cooling, a solution of methyl iodide (12 ml) in THF (35 ml) was added and kept overnight at room temperature. The crude product obtained after the usual work-up was chromatographed to give 6-methoxy-1-hexanol. Yield; 8.16 g. kept at 60° C. until gas evolution After cooling The crude product obtained after the usual work-up was chromatographed

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

実験手順: 6-Methoxy-hexanol (8.16 g) was oxidized with Jones reagent (2.67-M, 53 ml) in acetone (100 ml) at -10° C. to give 6.17 g of 6-methoxy-caproic acid.

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

実験手順: Sodium hydride (NaH) (50%, 6.12 g) suspended in tetrahydrofuran (TEF) (60 ml) was added to a solution of 1,6-hexanediol (15.0 g) in THP (200 ml), and kept at 60° C. until gas evolution stopped. After cooling, a solution of methyl iodide (12 ml) in THF (35 ml) was added and kept overnight at room temperature. The crude product obtaind after the usual work-up was chromatographed to give 6-methoxy-1-hexanol. Yield; 8.16 g kept at 60° C. until gas evolution After cooling The crude product obtaind after the usual work-up was chromatographed

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

実験手順: Sodium hydride (NaH) (50%, 6.12 g) suspended in tetrahydrofuran (TEF) (60 ml) was added to a solution of 1,6-hexanediol (15.0 g) in THP (200 ml), and kept at 60° C. until gas evolution stopped. After cooling, a solution of methyl iodide (12 ml) in THF (35 ml) was added and kept overnight at room temperature. The crude product obtaind after the usual work-up was chromatographed to give 6-methoxy-1-hexanol. Yield; 8.16 g kept at 60° C. until gas evolution After cooling The crude product obtaind after the usual work-up was chromatographed

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

実験手順: 803.6 grams of the monomethyl ether described in Part (A) above were azeotropically esterified with 629.8 grams acrylic acid in 254.6 grams toluene in the presence of 24 grams p-toluenesulfonic acid and inhibitors until no more water was collected. Conditions were 95°-98° C., nitrogen sparge in vacuo. On completion, the product was washed and neutralized with sodium carbonate. 900 ppm p-methoxyphenol (MEHQ) was added and the solvent removed at 80° C. with maximum vacuum in the presence of an air sparge. Filter aid was added and the product filtered at 60° C. to give a clear, yellow liquid having a viscosity of 6.5 cps and a Gardener color of 3. Equipment used was a 2 liter flask, thermometer, Dean-Stark condenser and sparge tube. was collected were 95°-98° C. nitrogen sparge in vacuo On completion, the product was washed 900 ppm p-methoxyphenol (MEHQ) was added the solvent removed at 80° C. with maximum vacuum in the presence of an air sparge Filter aid was added the product filtered at 60° C. to give a clear, yellow liquid thermometer, Dean-Stark condenser and sparge tube

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

実験手順: 803.6 grams of the monomethyl ether described in Part (A) above were azeotropically esterified with 629.8 grams acrylic acid in 254.6 grams toluene in the presence of 24 grams p-toluenesulfonic acid and inhibitors until no more water was collected. Conditions were 95°-98° C., nitrogen sparge in vacuo. On completion, the product was washed and neutralized with sodium carbonate. 900 ppm p-methoxyphenol (MEHQ) was added and the solvent removed at 80° C. with maximum vacuum in the presence of an air sparge. Filter air was added and the product filtered at 60° C. to give a clear, yellow liquid having a viscosity of 6.5 cps and a Gardener color of 3. Equipment used was a 2 liter flask, thermometer, Dean-Stark condenser and sparge tube. was collected were 95°-98° C. nitrogen sparge in vacuo On completion, the product was washed 900 ppm p-methoxyphenol (MEHQ) was added the solvent removed at 80° C. with maximum vacuum in the presence of an air sparge Filter air was added the product filtered at 60° C. to give a clear, yellow liquid thermometer, Dean-Stark condenser and sparge tube