Hydrogen Peroxide → HCID 86600860, compound

Temperature

0 °C

To a stirred solution of the product from Step D (2.77 g, 6.23 mmol) in THF (60 mL) was added water (20 mL). The solution was stirred at 0° C. for 15 min, and then 30% hydrogen peroxide (6.0 mL, 52.9 mmol) was added followed by slow addition of lithium hydroxide (0.50 g, 21.2 mmol). The resultant mixture was stirred at 0° C. for 4 h. The reaction was quenched by addition of saturated aqueous sodium sulfite solution and stirred at room temperature for 30 min. The aqueous phase was separated and washed with three portions of dichloromethane. The aqueous phase was then acidified to pH 1 with 3N hydrochloric acid and extracted with three portions of ethyl acetate. The ethyl acetate extracts were combined, dried over sodium sulfate, and evaporated in vacuo to give the product, which was used in the next step directly.

1. customThe reaction was quenched by addition of saturated aqueous sodium sulfite solution
2. stirringstirred at room temperature for 30 min
3. customThe aqueous phase was separated
4. washwashed with three portions of dichloromethane
5. extractionextracted with three portions of ethyl acetate
6. dry with materialdried over sodium sulfate
7. customevaporated in vacuo
8. customto give the product, which

ORD record

ord-d252e9afef084e6492253d592e4eaf5b

Source dataset

uspto-grants-2007_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07157490B2