2-Hydroxyethanesulphonic acid synthesis
- Product Name:2-Hydroxyethanesulphonic acid
- CAS Number:107-36-8
- Molecular formula:C2H6O4S
- Molecular Weight:126.13
1562-00-1
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Yield:107-36-8 91.1%
Reaction Conditions:
with hydrogenchloride in isopropyl alcohol at 20 - 50;
Steps:
10
EXAMPLE 10 Preparation of isethionic acid (2-HYDROXY-ETHANESULFONIC acid) A 5-L, four-necked, round-bottomed flask, equipped with mechanical stirrer, thermocouple, gas sparger, and an atmosphere vent through a water trap was charged with 748 g (5. 05 mol) of sodium isethionate (ALDRICH), and 4 L of IPA. The SLURRY was stirred at RT. An ice bath was used to keep the internal temperature below 50°C as 925 g (25. 4 mol) of hydrogen chloride gas (ALDRICH) was sparged into the system at a rate such that it dissolved as fast as it was added (as noted by lack of bubbling through the water trap). Sufficient HCI gas was added until the system was saturated (as noted by the start of bubbling through the water trap). During the addition of HCI, the temperature rose to 45°C. The slurry was cooled to RT and filtered over a COARSE-FRITTED filter. The cake was washed with 100 mL of IPA and the. cloudy filtrate was filtered through a 10-20μ filter. The resulting clear, colorless filtrate was concentrated under reduced pressure on a rotary evaporator, while keeping the bath temperature below 50°C. The resulting 1.07 kg of clear, light yellow oil was diluted with 50 mL of tap water and 400 mL of toluene and concentrated under reduced pressure on a rotary evaporator for three days, while keeping the bath temperature below 50°C. The resulting 800 g of clear, light yellow oil was diluted with 500 mL of toluene and 250 mL of IPA and concentrated under reduced pressure on a rotary evaporator for 11 days, keeping the bath temperature below 50°C. The resulting 713 g of clear, light yellow oil was titrated at 81 wt % (580 g, 91. 1% yield) containing 7.9 wt % water and 7.5 wt % IPA.
References:
WO2005/5426,2005,A1 Location in patent:Page/Page column 24; 25
5324-47-0
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1184-84-5
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