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ChemicalBook CAS DataBase List BIS(T-BUTYLDIMETHYLSILOXY)ETHANE

BIS(T-BUTYLDIMETHYLSILOXY)ETHANE synthesis

2synthesis methods
18162-48-6 Synthesis
tert-Butyldimethylsilyl chloride

18162-48-6
655 suppliers
$9.00/5g

102229-10-7 Synthesis
(TERT.-BUTYLDIMETHYLSILYLOXY)ETHANOL

102229-10-7
171 suppliers
$10.00/1g

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Yield: 13.7 g

Reaction Conditions:

with pyridine in hexane at 20; for 0.5 h;Temperature;Solvent;

Steps:

5
The 13g of tert-butyldimethylsilyl chloride were added to 26.1g of dichloromethane, stirred to dissolution, to give tert-butyldimethylsilyl chloride in dichloromethane solution; 52.2g was added to the reaction apparatus B diol, 78.3 g of methylene chloride and 36.7g of pyridine, cooled to -30 deg.] C, added dropwise tert-butyldimethylsilyl chloride in methylene chloride dropwise reaction was continued for 30min.After completion of the reaction, added at a concentration of 10wt% phosphate - monobasic potassium phosphate buffer adjusted to pH 2 the reaction system, and then with saturated brine the reaction system pH was adjusted to 6, stand, collect the organic phase, adding a drying agent, filtered and concentrated to give 16.9g of 2- (tert-butyldimethylsilyloxy) ethanol, weight yield 130%, GC content of 85.0% is detected, the molar yield of 94.5%, GC content of byproducts detected disubstituted 3.45% . The method of each comparative example is basically the same as that of Embodiment 1 except that step is described in detail

References:

Changzhou Lanling Pharmaceutical Co., Ltd.;Xu Fangfang;Wu Wenqiang CN107417718, 2017, A Location in patent:Paragraph 0023; 0024

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