2,4-Diethyl-9H-thioxanthen-9-one synthesis
- Product Name:2,4-Diethyl-9H-thioxanthen-9-one
- CAS Number:82799-44-8
- Molecular formula:C17H16OS
- Molecular Weight:268.37
141-93-5
124 suppliers
$44.00/2ml
119-80-2
425 suppliers
$7.00/25g
82799-44-8
281 suppliers
$5.00/5g
Yield:82799-44-8 90.2%
Reaction Conditions:
with sulfuric acid at 0 - 65; for 6 h;Reagent/catalyst;
Steps:
1-2 Example one
Add 40 ml of concentrated sulfuric acid to a 500 ml four-neck reaction flask.100 grams of dithiosalicylic acid,8 grams of polyphosphate,With stirring in an ice-salt bath to cool below 0 ° C, 100 g of 1,3-diethylbenzene was added dropwise to control the reaction temperature not to exceed 5 ° C.After the addition was completed, the ice-salt bath was removed, the temperature was naturally raised to room temperature, and the reaction was continued for 1 hour.The oil bath was replaced, the temperature was slowly raised to 65 ° C, and the reaction was performed at 65 ° C for 5 hours. The reaction was followed by HPLC until the dithiosalicylic acid reaction was completed.The reaction product was cooled, 90 g of 1,3-diethylbenzene and 60 g of water were added, and the mixture was stirred for half an hour, and the phases were separated. The organic phase was washed with alkali, washed with water, concentrated, and then cooled to 5 ° C.Overnight, the next day was filtered, the filter cake was washed with a small amount of ice ethanol, and dried in vacuum.150 g of bright yellow crystalline powder, namely DETX finished product,Yield 90.2%,Melting point 71 72 ,The purity of the product by HPLC was 99.6%.
References:
Ji'an Dongqing Fine Chemical Co., Ltd.;Ceng Xiaojun CN110845471, 2020, A Location in patent:Paragraph 0008; 0027-0030
141-93-5
124 suppliers
$44.00/2ml
119-80-2
425 suppliers
$7.00/25g
98-07-7
327 suppliers
$13.00/25g
82799-44-8
281 suppliers
$5.00/5g
