Water → 2,3,5-Triiodobenzyl mesylate

Mesyl chloride (0.6 ml, 8 mmol) was added dropwise to a suspension of 2,3,5-triiodobenzyl alcohol 1 (1.94 g, 4 mmol) in dry dichloromethane (30 ml) containing diisopropylethylamine (1.4 ml, 8 mmol) at 0° C. under dry nitrogen gas flow. The reaction mixture was stirred 1 h15 at 0° C., then cold H2O (40 ml) was added. The resulting aqueous phase was extracted with dichloromethane (10 ml). The combined organic extracts were washed with H2O (8 ml) then dried (Na2SO4), filtered and concentrated. The pale yellow solid was also washed with cold methanol (35 ml). 1.894 g of 2,3,5-triiodobenzyl mesylate in the form of a white clean solid was obtained in 84% yield.

1. extractionThe resulting aqueous phase was extracted with dichloromethane (10 ml)
2. washThe combined organic extracts were washed with H2O (8 ml)
3. dry with materialthen dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated
6. washThe pale yellow solid was also washed with cold methanol (35 ml)

ORD 기록

ord-b3c177c46c9440bfbfacdcf93b922d39

출처 데이터셋

uspto-grants-2015_08

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US09115230B2