ChemicalBook CAS DataBase List 2-Phenyl-2-propyl benzodithioate

2-Phenyl-2-propyl benzodithioate synthesis

5synthesis methods

Product Name:2-Phenyl-2-propyl benzodithioate
CAS Number:201611-77-0
Molecular formula:C16H16S2
Molecular Weight:272.43

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98-83-9 Synthesis

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201611-77-0
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Yield:-

Reaction Conditions:

with hydrogenchloride in n-heptane;water;

Steps:

4 EXAMPLE 4

[0081] 32 g of sulfur powder were added to 432 g of a 12% sodium methoxide solution. 63 g of benzoyl chloride were added dropwise to this solution with stirring over 1 hour. The temperature rose to 43° C., and a brown coloration occurred. After all the benzoyl chloride had been added, the reaction mixture was heated to 67° C. for 5 hours, then cooled to 7° C. A precipitate formed and was removed from the reaction mixture by filtration. The precipitate was washed with methanol, after which the methanol was removed with the aid of a rotary evaporator. [0082] The solid obtained was transferred into a 500 ml separating funnel with the aid of 400 ml of water. The aqueous solution was extracted with three 50 ml portions of toluene. 188.2 g of the aqueous solution obtained (containing approx. 0.173 mol of sodium dithiobenzoate) were transferred into a 250 ml separating funnel. 20.5 g of α-methylstyrene and 30 ml of heptane were added thereto. Portions of 37% aqueous hydrochloric acid were added thereto, shaking vigorously after each addition. The hydrochloric acid addition was continued until the aqueous phase was virtually colorless and had a pH of less than 7. The organic phase was extracted using 2% aqueous sodium hydroxide solution. Volatile materials were then removed. 31.5 g of a deep violet oil were obtained.

References:

US2004/186302,2004,A1 Location in patent:Page 5