Organic Syntheses by Unknown
page 35 of 106 (33%)
page 35 of 106 (33%)
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The 875 g. of dichlorohydrin thus obtained boils over a
7'0 range; this is 70 per cent of the theoretical amount. Redistillation yields 700-720 g. boiling 70-73'0/14 mm. (57 per cent of the theoretical amount). 2. Notes The most convenient hydrogen chloride generator is that described by Sweeney.[1] Concentrated hydrochloric acid is introduced into concentrated sulfuric acid, by means of a dropping funnel and a _capillary tube leading to the bottom of the sulfuric acid container_. It is convenient to use a 3-l. bottle for this container and a 1-l. funnel to contain the hydrochloric acid. The gas is dried by passing through a wash-bottle containing concentrated sulfuric acid. An empty catch-flask should be connected between the generator and the absorption flask in case any glycerol tends to suck back at the start of the reaction. About 6 kg. of concentrated hydrochloric acid and 10 kg. of concentrated sulfuric acid are required in one run. The generating flask will have to be recharged every six hours; it should be half filled with sulfuric acid. Aside from this, the apparatus needs no attention. The oil bath can be conveniently heated on an electric hot plate. The dichlorohydrin boiling over a 7'0 range is sufficiently pure for most purposes. It contains very little, if any, isomeric dichlorohydrin, since on oxidation it gives dichloroacetone in good yields. |
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