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5-fluoro-4-(2-methyl-1-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-5-yl)pyrimidin-2-amine → 5-Fluoro-N-(2-fluoro-4-(morpholinomethyl)phenyl)-4-(2-methyl-1-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-5-yl)pyrimidin-2-amine

HRID 31
ノート
印刷プレビュー

反応式

HRID 31 の反応式
Cc1ncc(-c2nc(N)ncc2F)n1C1CCOCC1.Fc1cc(CN2CCOCC2)ccc1Cl>C1COCCO1.CC(C)(C)[O-].CC(C)c1cc(C(C)C)c(-c2ccccc2P(C2CCCCC2)C2CCCCC2)c(C(C)C)c1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.[K+].[Pd].[Pd]>Cc1ncc(-c2nc(Nc3ccc(CN4CCOCC4)cc3F)ncc2F)n1C1CCOCC1
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 166654985-fluoro-4-(2-methyl-1-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-5-yl)pyrimidin-2-amineHCID 595438604-(4-Chloro-3-fluorobenzyl)morpholine

生成物 1

HCID 497820135-Fluoro-N-(2-fluoro-4-(morpholinomethyl)phenyl)-4-(2-methyl-1-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-5-yl)pyrimidin-2-amine収率 11.43%

試薬・触媒・溶媒 4

HCID 23665647Potassium tert-butoxide試薬
HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
102 °C

実験手順

To degassed 1,4-dioxane (39.2 ml) in a flame-dried and argonflushed 250 mL roundbottomed flask were added 5-fluoro-4-(2-methyl-1-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-5-yl)pyrimidin-2-amine (1.076 g, 3.88 mmol) and 4-(4-chloro-3-fluorobenzyl)morpholine (0.9 g, 3.92 mmol) followed by POTASSIUM TERT-BUTOXIDE (0.572 g, 5.09 mmol) whilst stirring. The resulting slurry was flushed with argon and stirred for 5-10 minutes followed by addition of TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (0.359 g, 0.39 mmol) and 2-Dicyclohexylphosphino-2',4',6'-tri-iso- propyl-1,1'-biphenyl (0.374 g, 0.78 mmol), whereafter the reaction mixture was flushed with argon again and heated to 102 °C and stirred under argon for 3 h. No further conversion occurred after 2 hours. The completion of the reaction was controlled by HPLC and the crude mixture was cooled to ambient temperatuer and then filtrated through Celite and washed through with dichloromethane. The solution was concentrated in vacuo and dissolved in 14 ml dichloromethane and purified by ISCO and then by prep-HPLC. The pooled fractions were concentrated in vacuo and added HCl to give 5-fluoro-N-(2-fluoro-4-(morpholinomethyl)phenyl)-4-(2-methyl-1-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-5-yl)pyrimidin-2-amine (0.227 g, 11.43 %)

出典と根拠

ORDレコード
ord-68a2d19644de420ea283722f281ee146
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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このページの内容参加物反応条件実験手順出典と根拠反応ノート