反応 #2042

反応方程式

triethylamine

Bis(5 -cyclohexyl-4-hydroxy-2-methylphenyl)-3,4-dihydroxyphenylmethane

methanesulfonyl chloride

→

bis(5-cyclohexyl-4-hydroxy-2-methylphenyl)-3,4-dihydroxyphenylmethane

methanesulfonic acid

溶媒

dioxane

dioxane

反応条件

後処理

1. 1
   workup.DISSOLUTIONdissolved
2. 2
   workup.ADDITIONtherein was added dropwise over 40 minutes at a controlled temperature not higher than 35° C
3. 3
   その他The precipitating salt was separated by filtration
4. 4
   その他the thus recovered reaction product
5. 5
   洗浄was washed
6. 6
   その他dried

実験手順

Bis(5 -cyclohexyl-4-hydroxy-2-methylphenyl)-3,4-dihydroxyphenylmethane(1.0 mole), naphthoquinone-1,2-diazido-5-sulfonyl chloride (2.0 moles) and methanesulfonyl chloride(0.5 moles) were dissolved in dioxane (4,000 g). To the resulting solution, dioxane (1,500 g) having triethylamine (500 g) dissolved therein was added dropwise over 40 minutes at a controlled temperature not higher than 35° C. The precipitating salt was separated by filtration and the thus recovered reaction product was washed and dried to yield a mixed ester of bis(5-cyclohexyl-4-hydroxy-2-methylphenyl)-3,4-dihydroxyphenylmethane with naphthoquinone-1,2-diazido-5-sulfonic acid and methanesulfonic acid; the average degree of esterification was 50% for the quinonediazidosulfonate ester and 12% for the methanesulfonate ester.

出典