Toluene → HCID 57293177、化合物

温度

-20 °C

A solution of 2,2-dimethyl-5-hydroxymethyl-5-methyl-1,3-dioxane (13.4 g, 0.084 mol) in 630 mL of anhydrous tetrahydrofuran was cooled to -20° C. under argon atmosphere. Then a 0.5M solution of potassium bis(trimethylsilyl)amide in toluene (168 mL, 0.084 mol) was added and the mixture was stirred at -20° C. for 1 hr. The 2-benzyloxyethyltriflate (23.8 g, 0.084 mol) was added neat, keeping the temperature between -20° and -15° C. The resulting solution was stirred at this temperature for 1 hr, then gradually allowed to warm to 25° C. and stirred for 15 hrs. Dichloromethane (900 mL) was added and the solution was washed twice with 300 mL of water and once with 100 mL of saturated sodium chloride solution. The organic layer was dried over anhydrous sodium sulfate and evaporation of the solvents under reduced pressure gave 2,2-dimethyl-5-benzyloxyethoxymethyl-5-methyl-1,3-dioxane (24.6 g, 0.084 mol, 100%) which was not purified.

1. customthe temperature between -20° and -15° C
2. stirringThe resulting solution was stirred at this temperature for 1 hr
3. temperatureto warm to 25° C.
4. stirringstirred for 15 hrs
5. washthe solution was washed twice with 300 mL of water and once with 100 mL of saturated sodium chloride solution
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate and evaporation of the solvents under reduced pressure

ORDレコード

ord-ce6759d5b59c49ff9fe8c980a9e44a64

出典データセット

uspto-grants-1995_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05417959