8-amino-2-methyl-3,4-dihydroisoquinolin-1(2H)-one → 8-[(2,5-Dichloropyridin-4-yl)amino]-2-methyl-3,4-dihydroisoquinolin-1-one

HRID 23

반응식

HRID 23 반응식
CN1CCc2cccc(N)c2C1=O.Clc1cc(I)c(Cl)cn1>C1COCCO1.CC(=O)O.CC(=O)O.CC1(C)c2cccc(P(c3ccccc3)c3ccccc3)c2Oc2c(P(c3ccccc3)c3ccccc3)cccc21.O=C([O-])[O-].[Cs+].[Cs+].[Pd]>CN1CCc2cccc(Nc3cc(Cl)ncc3Cl)c2C1=O

참가 물질

7

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온도
100 °C

실험 절차

diacetoxypalladium (24.59 mg, 0.11 mmol) was added to a stirred suspension of 2,5-dichloro-4-iodopyridine (600 mg, 2.19 mmol), 8-amino-2-methyl-3,4-dihydroisoquinolin-1(2H)-one (386 mg, 2.19 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (127 mg, 0.22 mmol) and cesium carbonate (1071 mg, 3.29 mmol) in 1,4-dioxane (10 mL). The resulting suspension was degassed with nitrogen and was stirred at 100 °C for 18 hours. Reaction was allowed to cool to room temperature, quenched with water and extracted with EtOAc. Combined organic phases were washed with water, brine, dried over MgSO4 and concentrated to dryness. The crude product was purified by flash chromatography on silica gel eluting with 0 to 10% ethyl acetate in dichloromethane. The solvent was evaporated to dryness to afford 8-(2,5-dichloropyridin-4-ylamino)-2-methyl-3,4-dihydroisoquinolin-1(2H)-one (447 mg, 63.3 %) as a pale yellow crystalline solid.

출처 및 근거

ORD 기록
ord-702aadae7425481bab668d630b5a0a21
출처 데이터셋
750 AstraZeneca ELN dataset
원본 링크
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