1-chloroethyl sulfochloridate synthesis
- Product Name:1-chloroethyl sulfochloridate
- CAS Number:90906-61-9
- Molecular formula:C2H4Cl2O3S
- Molecular Weight:179.02
50893-53-3
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Yield:90906-61-9 90%
Reaction Conditions:
with chlorosulfonic acid in dichloromethane at 0; for 4 h;Inert atmosphere;
Steps:
1.1A 1A: l-Chloroethyl chlorosulfate
To a stirred solution of l-chloroethyl chloroformate (3.02 mL, 28.0 mmol) in dry dichloromethane (40 mL) at 0 °C, chlorosulfonic acid (3.72 mL, 56.0 mmol) was added slowly for 10 min. The reaction mixture was stirred at 0 °C for 4 h under nitrogen atmosphere. The reaction mixture was quenched with ice water and extracted with dichloromethane (200 mL). The organic layer was washed with 10% sodium bicarbonate solution and brine solution, dried over anhydrous sodium sulphate and concentrated under vacuum at ~30 °C to give l-chloroethyl chlorosulfate (4.500 g, 25.1 mmol, 90%) as a light yellowish liquid. NMR (300 MHz, chloroform-if) d ppm = 6.54 - 6.42 (m, 1H), 2.00 (d, =6.0 Hz, 3H).
References:
WO2019/136112,2019,A1 Location in patent:Page/Page column 43; 44
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