(3R-trans)-[2-[3,5-Bis[[(1,1-diMethylethyl)diMethylsilyl]oxy]cyclohexylidene]ethyl]diphenyl-phosphine Oxide synthesis
- Product Name:(3R-trans)-[2-[3,5-Bis[[(1,1-diMethylethyl)diMethylsilyl]oxy]cyclohexylidene]ethyl]diphenyl-phosphine Oxide
- CAS Number:139356-39-1
- Molecular formula:C32H51O3PSi2
- Molecular Weight:570.89
Yield: 80%
Reaction Conditions:
Stage #1:diphenylphosphane with n-butyllithium in tetrahydrofuran at 0; for 0.5 h;
Stage #2:((1R,3R)-5-(2-chloroethylidene)cyclohexane-1,3-diyl)bis(oxy)bis(tert-butyldimethylsilane) in tetrahydrofuran for 3 h;
Steps:
11 Example 10: Preparation of Compound I.
Compound II (38.6 g, 0.1 mol) was dissolved in 500 mL dry DMF and pyridine (31.6 g, 0.4 mol) and anhydrous lithium chloride (17 g, 0.4 mol) were added and cooled to 0 ° C. Methanesulfonyl chloride 23g, 0.2mol) was added. The mixture was stirred for 2h. No residue of raw material was detected by TLC. The mixture was quenched with 500mL of water and extracted with methyl tert-butyl ether. The dry compound III was concentrated by drying and dissolved in 500mL of dry THF.N-Butyllithium (200 mL, 0.5 mol) was added to a THF solution of diphenylphosphine (93 g, 0.5 mol) at 0 ° C and stirred for 30 min. The THF solution of Compound III was added dropwise to the reaction mixture and stirred for 3 h , TLC no raw material, water, stirred 20min, 200mL 30% H2O2 was added and stirred for 2h, extracted, dried and concentrated to give the crude product, which was purified by silica gel column chromatography to obtain 45.6g of compound I, yield 80%.
References:
Shanghai Haoyuan Pharmaceutical Co., Ltd.;Li Hongkun;Ding Fudou;Sun Min;Zhang Xianshu;Gao Qiang;Zheng Baofu CN107501317, 2017, A Location in patent:Paragraph 0084; 0085; 0086; 0087
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