Hydrogen Peroxide → 6-Hydroxy-5-methyl-4-(4-phenoxy-phenylamino)-pyrrolo[1,2-b]pyridazine-3-carbonitrile

温度

-10 °C

34% H2O2 (53 μl, 0.058 mmol) was added to CH2Cl2 (3 ml) at −10° C., then BF3.Et2O (0.64 ml, 5.0 mmol) was added. After the mixture was stirred at −10° C. for 20 min, a suspension of 396 (165 mg, 0.42 mmol) in CH2Cl2 (2 ml) was added. The reaction was stirred at −10° C. for 5 min, then quenched with aq Na2SO3, extracted with EtOAc. The organic layer was dried, concentrated and purified by silica gel flash column chromatography to give 397A (125 mg, 85%) (10% EtOAc—CH2Cl2).

1. additionwas added
2. stirringThe reaction was stirred at −10° C. for 5 min
3. customquenched with aq Na2SO3
4. extractionextracted with EtOAc
5. customThe organic layer was dried
6. concentrationconcentrated
7. custompurified by silica gel flash column chromatography

ORDレコード

ord-2a88b91133454ef98c505e5c118fd0ae

出典データセット

uspto-grants-2006_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07030112B2