三氯-lambda3-碘烷

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To 200 ml of acetone were added 10.0 g of L-sorbose and 234 mg of iodine trichloride and the mixture was refluxed with stirring in a water bath at 60° C. for 4 hours. During this reaction, the refluxing solvent was dried with 20 g of Molecular Sieves 3A interposed between the reaction vessel and the cooling jacket. The reaction mixture was then subjected to an after-treatment similar to that described in Example 11 to give 9.85 g (68.2%) of 2,3:4,6-di-O-isopropylidene-L-sorbofuranose (purity ≥98%). the mixture was refluxed During this reaction the refluxing solvent was dried with 20 g of Molecular Sieves 3A

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To 200 ml of acetone were added 10.0 g of L-sorbose and 234 mg of iodine trichloride and the mixture was refluxed with stirring in a water bath at 60° C. for 4 hours. During this reaction, the refluxing solvent was dried with 20 g of Molecular Sieves 3A interposed between the reaction vessel and the cooling jacket. The reaction mixture was then subjected to an after-treatment similar to that described in Example 11 to give 9.85 g (68.2%) of 2,3:4,6-di-O-isopropylidene-L-sorbofuranose (purity ≥98%). the mixture was refluxed During this reaction the refluxing solvent was dried with 20 g of Molecular Sieves 3A

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

实验步骤: 203 parts of 2,4-dinitrochlorobenzene (setting point 49° C.) are saponified to 2,4-dinitrophenol in a mixture of 303 parts of 33% strength sodium hydroxide solution and 200 parts of water at 95° C. under a nitrogen atmosphere. The resulting suspension is adjusted to a pH value of 3.5 by adding 185 parts of 31% strength hydrochloric acid. After 10 parts of the sodium salt of a naphthalenesulfonic acid/formaldehyde condensation product (dispersing agent), 1 part of iron(III) chloride and 1 part of iodine trichloride have been added, 650 parts of 13 percent strength by weight chlorine bleach liquor (containing 150 parts of active chlorine per liter) are added dropwise at 10° C. in the course of 8 hours, the pH increasing meanwhile. Towards the end of the addition, the pH reaches a value of 6. After it has reached this value, the pH is kept at this value (pH 6) by the simultaneous dropwise addition of 5-20 parts of 31% strength hydrochloric acid and the remainder of the chlorine bleach liquor. The pH of the suspension is then adjusted to a value of 1.0 by adding 170 parts of 31% strength hydrochloric acid, and small amounts of sodium hypochlorite still present are destroyed by means of 15 parts of 40% strength sodium bisulfite solution. The resulting product is then isolated by being filtered off at about 10° C. This gives only 130 parts of 6-chloro-2,4-dinitrophenol with a black-brown appearance and a content of unsaponified 2,4-dinitrochlorobenzene which is clearly detectable in a thin layer chromatogram. have been added are added dropwise at 10° C. in the course of 8 hours the pH increasing meanwhile Towards the end of the addition still present are destroyed by means of 15 parts of 40% strength sodium bisulfite solution The resulting product is then isolated by being filtered off at about 10° C

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

实验步骤: A mixture of 183 parts of 2,4-dinitrochlorobenzene, 16 parts of 2,4-dinitrophenol and 3 parts of 2,4-dinitromethoxyethoxybenzene is saponified to 2,4-dinitrophenol in a mixture of 303 parts of 33% strength sodium hydroxide solution and 3,000 parts of water at 95° C. under an atmosphere of air. The resulting suspension i adjusted to a pH value of 3.5 by adding 185 parts of 31% strength hydrochloric acid. After 10 parts of the sodium salt of a naphthalenesulfonic acid formaldehyde condensation product (dispersing agent), 1 part of iron(III) chloride and 1 part of iodine trichloride have been added, 650 parts of 13 percent strength by weight chlorine bleach liquor (containing 150 g of active chlorine per liter) are added dropwise at 10° C. in the course of 8 hours, the pH increasing meanwhile. In the course of the addition, the pH reaches a value of 4.5. After it has reached this value, the pH is caused to remain, during the chlorination, within the range 4-4.5 by the simultaneous addition of 36 parts of 31% strength hydrochloric acid during the dropwise addition of the remainder of the chlorine bleach liquor. The pH of the suspension is then adjusted to a value of 1.0 by means of 170 parts of 31% strength hydrochloric acid, and small amounts of sodium hypochlorite still present are destroyed by means of 15 parts of 40% strength sodium bisulfite solution. The resulting product is then isolated by being filtered off at about 10° C. 200 parts of pale yellow 6-chloro-2,4-dinitrophenol (melting point: 101°-109° C.), now only containing traces (0.5%) of 2,4-dinitrophenol, are obtained. have been added are added dropwise at 10° C. in the course of 8 hours the pH increasing meanwhile In the course of the addition still present are destroyed by means of 15 parts of 40% strength sodium bisulfite solution The resulting product is then isolated by being filtered off at about 10° C

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To 200 ml of acetone were added 10.0 g of L-sorbose and 234 mg of iodine trichloride and the mixture was refluxed with stirring in a water bath at 60° C. for 4 hours. During this reaction, the refluxing solvent was dried with 20 g of Molecular Sieves 3A interposed between the reaction vessel and the cooling jacket. The reaction mixture was then subjected to an after-treatment similar to that described in Example 11 to give 9.85 g (68.2%) of 2,3:4,6-di-O-isopropylidene-L-sorbofuranose (purity ≥98%). the mixture was refluxed During this reaction the refluxing solvent was dried with 20 g of Molecular Sieves 3A