甲基2,2,3,3,3-五氟丙基醚

反应条件: temp:33.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methyl 2,2,3,3,3-pentafluoropropyl ether (225g, 1.37 mole) in a flask fitted with a dry ice cooled condensor and moisture trap was stirred, heated to 33°C, irradiated with ultraviolet light, and sulfuryl chloride (174 g, 1.29 mole) was added dropwise. The reaction temperature dropped to about 0°C as SO2 returned from the condensor. The condensor was allowed to warm gradually to permit SO2 to escape and the reaction temperature to rise to about 33°C to complete the chlorination. The product was washed with ice cold water then with dilute sodium hydroxide solution to remove SO2 and dried to give 250 g of crude XXVII. This was fractionally distilled to give XXVII, b760 87.1-88.5; yield 159 g, purity 92% by GLC. The structure of XXVII was confirmed by proton NMR spectroscopy. was added dropwise The reaction temperature dropped to about 0°C as SO2 to warm gradually to rise to about 33°C The product was washed with ice cold water with dilute sodium hydroxide solution to remove SO2 dried

反应条件: temp:33.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methyl 2,2,3,3,3-pentafluoropropyl ether (225g, 1.37 mole) in a flask fitted with a dry ice cooled condensor and moisture trap was stirred, heated to 33°C, irradiated with ultraviolet light, and sulfuryl chloride (174 g, 1.29 mole) was added dropwise. The reaction temperature dropped to about 0°C as SO2 returned from the condensor. The condensor was allowed to warm gradually to permit SO2 to escape and the reaction temperature to rise to about 33°C to complete the chlorination. The product was washed with ice cold water then with dilute sodium hydroxide solution to remove SO2 and dried to give 250 g of crude XXVII. This was fractionally distilled to give XXVII, b760 87.1-88.5; yield 159 g, purity 92% by GLC. The structure of XXVII was confirmed by proton NMR spectroscopy. was added dropwise The reaction temperature dropped to about 0°C as SO2 to warm gradually to rise to about 33°C The product was washed with ice cold water with dilute sodium hydroxide solution to remove SO2 dried

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

实验步骤: The ether V can be prepared by a method analogous to that described by Weinmayr1, or from methyl 2,2,3,3,3-pentafluoropropyl ether and one molar equivalent of sulfuryl chloride at 0°-35°C with ultraviolet irradiation to give the chloromethyl 2,2,3,3,3-pentafluoropropyl ether XXVII,

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

实验步骤: The ether V can be prepared by a method analogous to that described by Weinmayr1, or from methyl 2,2,3,3,3-pentafluoropropyl ether and one molar equivalent of sulfuryl chloride at 0°-35°C with ultraviolet irradiation to give the chloromethyl 2,2,3,3,3-pentafluoropropyl ether XXVII,

反应条件: temp:33.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methyl 2,2,3,3,3-pentafluoropropyl ether (225g, 1.37 mole) in a flask fitted with a dry ice cooled condensor and moisture trap was stirred, heated to 33°C, irradiated with ultraviolet light, and sulfuryl chloride (174 g, 1.29 mole) was added dropwise. The reaction temperature dropped to about 0°C as SO2 returned from the condensor. The condensor was allowed to warm gradually to permit SO2 to escape and the reaction temperature to rise to about 33°C to complete the chlorination. The product was washed with ice cold water then with dilute sodium hydroxide solution to remove SO2 and dried to give 250 g of crude XXVII. This was fractionally distilled to give XXVII, b760 87.1-88.5; yield 159 g, purity 92% by GLC. The structure of XXVII was confirmed by proton NMR spectroscopy. was added dropwise The reaction temperature dropped to about 0°C as SO2 to warm gradually to rise to about 33°C The product was washed with ice cold water with dilute sodium hydroxide solution to remove SO2 dried

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

实验步骤: The ether V can be prepared by a method analogous to that described by Weinmayr1, or from methyl 2,2,3,3,3-pentafluoropropyl ether and one molar equivalent of sulfuryl chloride at 0°-35°C with ultraviolet irradiation to give the chloromethyl 2,2,3,3,3-pentafluoropropyl ether XXVII,

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

实验步骤: The ether V can be prepared by a method analogous to that described by Weinmayr1, or from methyl 2,2,3,3,3-pentafluoropropyl ether and one molar equivalent of sulfuryl chloride at 0°-35° C with ultraviolet irradiation to give the chloromethyl 2,2,3,3,3-pentafluoropropyl ether XXVII,

反应条件: temp:33.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methyl 2,2,3,3,3-pentafluoropropyl ether (225g, 1.37 mole) in a flask fitted with a dry ice cooled condensor and moisture trap was stirred, heated to 33°C, irradiated with ultraviolet light, and sulfuryl chloride (174 g, 1.29 mole) was added dropwise. The reaction temperature dropped to about 0°C as SO2 returned from the condensor. The condensor was allowed to warm gradually to permit SO2 to escape and the reaction temperature to rise to about 33°C to complete the chlorination. The product was washed with ice cold water then with dilute sodium hydroxide solution to remove SO2 and dried to give 250 g of crude XXVII. This was fractionally distilled to give XXVII, b760 87.1-88.5; yield 159 g, purity 92% by GLC. The structure of XXVII was confirmed by proton NMR spectroscopy. was added dropwise The reaction temperature dropped to about 0°C as SO2 to warm gradually to rise to about 33°C The product was washed with ice cold water with dilute sodium hydroxide solution to remove SO2 dried

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

实验步骤: The ether V can be prepared by a method analogous to that described by Weinmayr1, or from methyl 2,2,3,3,3-pentafluoropropyl ether and one molar equivalent of sulfuryl chloride at 0°-35°C with ultraviolet irradiation to give the chloromethyl 2,2,3,3,3-pentafluoropropyl ether XXVII,