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N-(4-chloropyridin-2-yl)cyclopropanecarboxamide → N-[4-[(6-Chloro-[1,3]dioxolo[4,5-B]pyridin-7-Yl)amino]-2-Pyridyl]cyclopropanecarboxamide

HRID 43
ノート
印刷プレビュー

反応式

HRID 43 の反応式
Nc1c(Cl)cnc2c1OCO2.O=C(Nc1cc(Cl)ccn1)C1CC1>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]>O=C(Nc1cc(Nc2c(Cl)cnc3c2OCO3)ccn1)C1CC1
参加物反応条件実験手順出典と根拠反応ノート

参加物

7

反応物 2

HCID 4394171N-(4-chloropyridin-2-yl)cyclopropanecarboxamideHCID 685486516-chloro-2H-[1,3]dioxolo[4,5-b]pyridin-7-amine

生成物 1

HCID 121232401N-[4-[(6-Chloro-[1,3]dioxolo[4,5-B]pyridin-7-Yl)amino]-2-Pyridyl]cyclopropanecarboxamide収率 43.73%

試薬・触媒・溶媒 4

HCID 10796Cesium carbonate試薬
HCID 636044
1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)
触媒
HCID 4144353Palladium (II) acetate触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
150 °C

実験手順

N-(4-chloropyridin-2-yl)cyclopropanecarboxamide (0.8 g, 4.07 mmol), 6-chloro-[1,3]dioxolo[4,5-b]pyridin-7-amine (0.702 g, 4.07 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (0.282 g, 0.49 mmol), diacetoxypalladium (0.046 g, 0.20 mmol) and cesium carbonate (2.65 g, 8.14 mmol) were suspended in 1,4-dioxane (15 mL) and sealed into a microwave tube. The reaction was heated to 150 °C for 30 minutes in the microwave reactor and cooled to RT. The reaction mixture was diluted with EtOAc (50 mL) and washed with water (50 mL). The organic layer was dried over MgSO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 0 to 100% EtOAc in isohexane. Pure fractions were evaporated to dryness to afford N-(4-(6-chloro-[1,3]dioxolo[4,5-b]pyridin-7-ylamino)pyridin-2-yl)cyclopropanecarboxamide (0.592 g, 43.7 %) as a white solid.

出典と根拠

ORDレコード
ord-43b38b44db094a5e90893913a2fe3478
出典データセット
750 AstraZeneca ELN dataset
元リンク
出典を表示

反応ノート

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