반응 #460067

반응 방정식

calcium chloride

hydrogen chloride

1-chloro-3-octanol

s-trioxane

→

3-chloromethoxy-1-chlorooctane

반응 조건

후처리

1. 1
   기타2 hours
2. 2
   기타The upper aqueous phase is removed by this action
3. 3
   기타The solid material is removed by filtration
4. 4
   workup.DISTILLATIONthe filtrate distilled

실험 절차

A slow stream of hydrogen chloride gas is passed into a mixture of 1-chloro-3-octanol (35.5 g., 0.218 mole) and s-trioxane (6.55 g., 0.073 mole) in a conical flask cooled to 0° C. and protected from atmospheric moisture. The process requires about 31/2 hours. The resulting two-phase mixture is treated with anhydrous calcium chloride at 25° C. for 64 hours. The upper aqueous phase is removed by this action. The solid material is removed by filtration and the filtrate distilled to give the 3-chloromethoxy-1-chlorooctane as a colorless liquid (28.2 g., 61%), b.p. 128°-130°/15 mm.; pmr (CDCl3) δ 0.88 (3H,t), 1.98 (2H,q), 3.61 (2H,t), 3.92 (H,m), and 5.51 (2H,s).

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