Ok, here's the full entry for the dibromodioxane, near verbatim:
METHOD #2: [128, 129]--To make dibromodioxane one stirs 500g dioxane in a flask which is in an ice bath, all of which is in the (fume) hood. 990g of liquid Br
2 is rapidly added, causing the solution to get hot (one can also bubble in an approximate amount of bromine from a gas canister). The solution is dumped into a bucket containing 2L of ice water, causing the immediate formation of a large mass of
orange dibromodioxane crystals which are seperated by vacuum filtration and dried."
"In an ice bath a flask containing 100g 1,3-benzodioxole or catechol or guaiacol and 200mL ether is stirred and then 200g dibromodioxane is slowly added so that the heat and reaction won't get out of control. After stirring for one hour the solution is poured into some water and the ether layer is seperated. The aqueous layer is extracted once with some more ether and the two ether fractions combined, dried with Na
2SO
4 and distilled to give bromo-benzeodioxole. (90%)"
References cited in the appendix:
CA, 47, 8032 (1953)
CA, 44, 8354 (1950)
Source: TSII, pg. 224 If you don't know, don't ask, because we won't tell.
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