1,2-庚二醇

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

实验步骤: A solution of 4.06 g. 4-hydroxymethyl-3-oxa-1-phenyl-nonan-1-ol 1-mono-p-toluene sulphonate (obtainable by reaction of styrene oxide with heptane-1,2-diol and partial tosylation of the 4-hydroxymethyl-3-oxa-1-phenylnonan-1-ols obtained) in 100 ml. phosphoric acid hexamethyltriamide is heated for 24 hours to 80°. One evaporates, works up as usual and obtains 2-phenyl-5-pentyl-1,4-dioxane as an oily isomer mixture. Isomerization of 1 g. of the mixture by 2 hours heating with 0.05 g. K tert.-butylate in 10 ml. dimethyl sulphoxide to 80° leads to trans-2-phenyl-5-pentyl-1,4-dioxane. obtained) in 100 ml One evaporates

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

实验步骤: A solution of the title B ketal (1.87 g, 11.8 mmol) in methanol (30 ml) and concentrated HCl (2.5 ml) was stirred at room temperature 3 hours. The solution was basified by adding concentrated NH4OH solution (10 ml) and the solvent was removed in vacuo. Saturated NaCl solution (50 ml) was added to the residue and the product was extracted into ether (4×50 ml). The combined ether extracts were washed with saturated NaCl solution (50 ml), dried (MgSO4) and freed of solvent in vacuo leaving the title C diol as a yellow oil (1.13 g, 81%) 13-C NMR consistent. TLC:silica gel, Et2O, vanillin, Rf =0.25.

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

实验步骤: Using 1,2-heptanediol, pyridine and p-toluenesulfonyl chloride, (RS)-1-p-toluenesulfonyloxy-2-heptanol 2c ##STR26## was prepared in the same manner as Example 1 of Production. was prepared in the same manner as Example 1 of Production

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

实验步骤: A solution of 4.06 g. 4-hydroxymethyl-3-oxa-1-phenyl-nonan-1-ol 1-mono-p-toluene sulphonate (obtainable by reaction of styrene oxide with heptane-1,2-diol and partial tosylation of the 4-hydroxymethyl-3-oxa-1-phenylnonan-1-ols obtained) in 100 ml. phosphoric acid hexamethyltriamide is heated for 24 hours to 80°. One evaporates, works up as usual and obtains 2-phenyl-5-pentyl-1,4-dioxane as an oily isomer mixture. Isomerization of 1 g. of the mixture by 2 hours heating with 0.05 g. K tert.-butylate in 10 ml. dimethyl sulphoxide to 80° leads to trans-2-phenyl-5-pentyl-1,4-dioxane. obtained) in 100 ml One evaporates