Water → HCID 59133000、化合物

温度

-10 °C

882.3 g of methoxymethyl triphenylphosphonium chloride was dispersed in 2600 mL of THF, and was cooled to −10° C. While keeping the internal temperature, 313.2 g of potassium-t-butoxide was added thereto. While keeping the internal temperature, the solution was stirred for 1 hour, and then THF (800 mL) solution containing 200.0 g of bicyclohexyl-4,4′-dione was added dropwise. While keeping the internal temperature, the solution was stirred for 1 hour, and then water was added to stop the reaction. The solvent was evaporated under reduced pressure. Then, the residue was added with hexane, was vigorously stirred, and was subjected to filtration (twice). The resultant product was mixed with the filtrate, then washed with 50% methanol aqueous solution and saturated saline in this order, and dried over anhydrous magnesium sulfate. The solvent was evaporated, to obtain 231.8 g of a white solid.

1. additionwas added
2. additionwas added dropwise
3. stirringthe solution was stirred for 1 hour
4. customthe reaction
5. customThe solvent was evaporated under reduced pressure
6. additionThen, the residue was added with hexane
7. stirringwas vigorously stirred
8. filtrationwas subjected to filtration (twice)
9. additionThe resultant product was mixed with the filtrate
10. washwashed with 50% methanol aqueous solution and saturated saline in this order
11. dry with materialdried over anhydrous magnesium sulfate
12. customThe solvent was evaporated

ORDレコード

ord-a6e1e44d925444beb2eaa4a288b12dc0

出典データセット

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08003006B2