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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 30
ノート
印刷プレビュー

反応式

HRID 30 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 9.15%

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 (13.900 ml) in a flame-dried and argonflushed 50 mL roundbottomed flask were added 5-fluoro-4-(2-methyl-1-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-5-yl)pyrimidin-2-amine (386 mg, 1.39 mmol) and 4-(4-chloro-3-fluorobenzyl)morpholine (320 mg, 1.39 mmol) followed by POTASSIUM TERT-BUTOXIDE (203 mg, 1.81 mmol) whilst stirring. The resulting slurry was flushed with argon followed by addition of TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (128 mg, 0.14 mmol) and 2-Dicyclohexylphosphino-2',4',6'-tri-iso-propyl-1,1'-biphenyl (200 mg, 0.42 mmol), whereafter the dark violet reaction mixture was again flushed with argon and heated to 102 °C and stirred under argon for 15 h. 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 a minimum amount of DMSO and purified via Preparative HPLC. The pooled fractions were concentrated in vacuo and added HCl. 5-fluoro-N-(2-fluoro-4-(morpholinomethyl)phenyl)-4-(2-methyl-1-(tetrahydro-2H-pyran-4-yl)-1H-imidazol-5-yl)pyrimidin-2-amine (60.0 mg, 9.15 %)

出典と根拠

ORDレコード
ord-2a024728550642b2b2e2724a7387802d
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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