Technology Process of C6H5SCH2B(OCH2)2
There total 1 articles about C6H5SCH2B(OCH2)2 which
guide to synthetic route it.
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synthetic route:
- Guidance literature:
-
In
hexane;
byproducts: water; water azeotrope was distilled from a hexane soln. of the boronic acid and HOCH2CH2OH, water was collected in a Dean-Stark trap; residual ethylene glycol was removed by treatment with anhyd. CaCl2, the ester was distilled under reduced pressure;
DOI:10.1021/om00074a005
- Guidance literature:
-
With
N,N,N,N,-tetramethylethylenediamine; sec.-butyllithium;
In
tetrahydrofuran;
sec-BuLi was added dropwise at -78°C to Me3SiCH2Cl in THF, TMEDAadded, stirred 45 min at -78°C, warmed to -55°C, boronatein THF was added, the mixt. was cooled to -78°C, warmed to 25°C overnight; 2 M ice-cold HCl was added, mixt. extd. with 5:1 Et2O-CH2Cl2, org. phase concd. in vacuo, residue was treated with HOCH2CH2OH and hexane or benzene, refluxed with a Dean-Stark trap, dried over CaCl2, evapd., residuedistilled in vacuo; elem. anal.;
DOI:10.1021/om00074a005
- Guidance literature:
-
With
hydrogenchloride;
In
tetrahydrofuran;
(Ar); to soln. of Me3SiCHLiCl was added boronic ester at -55°C, mixt. was cooled with dry ice, then allowed to warm up slowly to room temp. and stirred overnight; mixt. was treated with aq. HCl and extd. with ether/CH2Cl2 5:1; esters were treated with ethylene glycol and distd.; elem. anal.;
DOI:10.1016/S0022-328X(00)83500-7