Aluminum(III) Chloride → 4-[4-(2,4,6-trimethyl-phenylamino)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino]-benzonitrile

To a solution of 4-[7-benzyl-4-(2,4,6-trimethyl-phenylamino)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino]-benzonitrile (34 mg, 0.074 mmol) in 1,2-dichlorobenzene (1 mL) was added aluminum chloride (50 mg, 0.37 mmol). The reaction mixture was stirred at 160° C. for 2 h and cooled to room temperature. The mixture was poured into ice water and extracted with CHCl3 (2×10 mL). The combined organic solution was washed with brine (10 mL), dried with Na2SO4, and concentrated to dryness. Silica gel chromatography (CH2Cl2:Acetone=90:10) yielded 5 mg (19%) of 4-[4-(2,4,6-trimethyl-phenylamino)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino]-benzonitrile as a tan solid.

1. temperaturecooled to room temperature
2. extractionextracted with CHCl3 (2×10 mL)
3. washThe combined organic solution was washed with brine (10 mL)
4. dry with materialdried with Na2SO4
5. concentrationconcentrated to dryness

ORD 기록

ord-afd23c18d6ba43f38eac2117d4c34ff2

출처 데이터셋

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08354532B2