Methanesulfonyl chloride → HCID 53403083, Verbindung

Mesyl chloride (4.24 ml, 56 mmol) was added dropwise into a suspension of 2,3,5-triiodobenzyl alcohol 1 (9.72 g, 20 mmol) in dry dichloromethane (140 ml) containing diisopropylethylamine (11 ml, 64 mmol) and lithium chloride (4.24 g, 100 mmol) at 0° C. under dry nitrogen gas flow. The reaction mixture was stirred 5 h at room temperature, then cold H2O (100 mL) was added. The resulting aqueous phase was extracted with dichloromethane (2×10 ml). The combined organic extracts were washed with NaHCO3 aq (20 ml) and H2O (20 ml) then dried (Na2SO4), filtered and concentrated. The pale yellow solid was also washed with cold absolute ethanol (25 mL). 9.05 g of 2,3,5-triiodobenzyl chloride in the form of a white clean solid was obtained in 90% yield.

1. extractionThe resulting aqueous phase was extracted with dichloromethane (2×10 ml)
2. washThe combined organic extracts were washed with NaHCO3 aq (20 ml) and H2O (20 ml)
3. dry with materialthen dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. washThe pale yellow solid was also washed with cold absolute ethanol (25 mL)

ORD-Eintrag

ord-beb4959a595d43828ccf9a72c7d90e22

Quelldatensatz

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09434800B2