2-(二氟甲氧基)苯酚

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: 275 g of chlorodifluoromethane are passed into a solution of 100 g of pyrocatechol, 220 g of sodium hydroxide and 60 g of sodium dithionite in 500 ml of water and 400 ml of dioxane at 50°-55° C. analogously to L. N. Sedova et al., Zh. Org. Khim. 6, 568 (1970). After distillation at 61°-62° C./1.0-1.1 kPa, a mixture of 1,2-bis(difluoromethoxy)benzene and 2-difluoromethoxyphenol is obtained, the products being separated by chromatography on silica gel by means of cyclohexane/ethyl acetate (4:1). After distillation at 61°-62° C./1.0-1.1 kPa a mixture of 1,2-bis(difluoromethoxy)benzene

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

实验步骤: To an ice cold suspension of 2-(difluoromethoxy)phenol (6.54 g, 0.00408 mol), aluminum trichloride (0.0544 g, 0.000408 mol) and 1,1′-thiodibenzene (0.068 mL, 0.000408 mol) was added sulfuryl dichloride (3.61 mL, 0.0449 mmol) dropwise. The reaction was allowed to warm to room temperature and stirred for 16 hours. The reaction was diluted in dichloromethane (10.0 mL) and purified using silica gel column chromatography eluting with 0-20% EtOAc in heptane. The title compound was isolated as a colourless oil (2.33 g, 0.01195 mol, 29%). purified eluting with 0-20% EtOAc in heptane

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

实验步骤: To an ice cold suspension of 2-(difluoromethoxy)phenol (6.54 g, 0.00408 mol), aluminum trichloride (0.0544 g, 0.000408 mol) and 1,1′-thiodibenzene (0.068 mL, 0.000408 mol) was added sulfuryl dichloride (3.61 mL, 0.0449 mmol) dropwise. The reaction was allowed to warm to room temperature and stirred for 16 hours. The reaction was diluted in dichloromethane (10.0 mL) and purified using silica gel column chromatography eluting with 0-20% EtOAc in heptane. The title compound was isolated as a colourless oil (2.33 g, 0.01195 mol, 29%). purified eluting with 0-20% EtOAc in heptane

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

实验步骤: To an ice cold suspension of 2-(difluoromethoxy)phenol (6.54 g, 0.00408 mol), aluminum trichloride (0.0544 g, 0.000408 mol) and 1,1′-thiodibenzene (0.068 mL, 0.000408 mol) was added sulfuryl dichloride (3.61 mL, 0.0449 mmol) dropwise. The reaction was allowed to warm to room temperature and stirred for 16 hours. The reaction was diluted in dichloromethane (10.0 mL) and purified using silica gel column chromatography eluting with 0-20% EtOAc in heptane. The title compound was isolated as a colourless oil (2.33 g, 0.01195 mol, 29%). purified eluting with 0-20% EtOAc in heptane

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

实验步骤: 275 g of chlorodifluoromethane are passed into a solution of 100 g of pyrocatechol, 220 g of sodium hydroxide and 60 g of sodium dithionite in 500 ml of water and 400 ml of dioxane at 50°-55° C. analogously to L. N. Sedova et al., Zh. Org. Khim. 6, 568 (1970). After distillation at 61°-62° C./1.0-1.1 kPa, a mixture of 1,2-bis(difluoromethoxy)benzene and 2-difluoromethoxyphenol is obtained, the products being separated by chromatography on silica gel by means of cyclohexane/ethyl acetate (4:1). After distillation at 61°-62° C./1.0-1.1 kPa a mixture of 1,2-bis(difluoromethoxy)benzene