m-Chloroperbenzoic acid → HCID 58504127, Verbindung

3-Chloroperoxybenzoic acid (195 mg) was added to a 0° C. suspension of the compound prepared in Example 93 (100 mg) in dichloromethane (4 mL). The reaction was stirred one hour at room temperature. Diisopropylethylamine (0.669 mL) and the compound prepared in Example 9 (198 mg) were added and the mixture was stirred at room temperature for 18 hours. The reaction was diluted with ethyl acetate and sequentially washed with a saturated sodium bicarbonate solution and brine. The organics were dried over magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (concentrated aqueous ammonia:methanol:ethyl acetate=0.1:0.9:25) to obtain the title compound (51 mg) having the following physical data.

1. stirringthe mixture was stirred at room temperature for 18 hours
2. washsequentially washed with a saturated sodium bicarbonate solution and brine
3. dry with materialThe organics were dried over magnesium sulfate
4. concentrationconcentrated
5. customThe residue was purified by column chromatography on silica gel (concentrated aqueous ammonia:methanol:ethyl acetate=0.1:0.9:25)

ORD-Eintrag

ord-2b81f81d2e8242fe8832b0d95e813af3

Quelldatensatz

uspto-grants-2014_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08809538B2