3',6'-dichlorospiro[benzo[c][1,2]oxathiole-3,9'-xanthene] 1,1-dioxide synthesis
- Product Name:3',6'-dichlorospiro[benzo[c][1,2]oxathiole-3,9'-xanthene] 1,1-dioxide
- CAS Number:77545-45-0
- Molecular formula:C19H10Cl2O4S
- Molecular Weight:405.25
4424-03-7
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Yield:77545-45-0 56%
Reaction Conditions:
with trichlorophosphate at 105; for 18 h;
Steps:
Synthesis of DCSF
36.8 g of sulfofluorescein and 150 g of phosphorus oxychloride were added to a 200 mL three-neck flask.
The mixture was heated to 105° C. and was stirred at 105° C. for 18 hours.
Next, the obtained reaction solution was cooled to 20° C. for 1 hour.
The obtained reaction solution was added to a 2 L three-neck flask to which 1 L of water was added for 20 minutes while cooling the flask in a water bath at 20° C. such that the water temperature did not exceed 35° C.
After the addition, the reaction solution was stirred at 20° C. for 1 hour.
The obtained suspension was filtered, and the obtained crystals were washed with 200 mL of water once and then was washed with 200 mL of acetonitrile twice.
After washing, the crystals were dried by blowing air at 50° C. for 18 hours.
As a result, 22.7 g of dichloro sulfonphthalein (DCSF) was obtained (yield: 56%).
References:
US2018/371254,2018,A1 Location in patent:Paragraph 0319; 0322; 0323
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